Hair cleansing composition

Abstract

A hair wash composition comprising: a) 1 to 50 wt. % of a cleansing surfactant selected from the group consisting of anionic surfactants, zwitterionic or amphoteric surfactants, nonionic surfactants, and mixtures thereof; and b) 0.01 to 3 wt. % of defibrated primary cell wall material comprising cellulose microfibrils, based on the total weight of the composition, wherein the defibrated primary cell wall material comprises up to 20 wt. % water, based on the total weight of the fibrils; the cellulose has an average crystallinity of less than 50%; and the defibrated primary cell wall material comprises a polyol distributed between the fibrils.

Description

[Technical Field]

[0001] The present invention relates to a hair cleansing composition comprising defibrated primary cell wall material comprising cellulose microfibrils, wherein the cellulose has a crystallinity of less than 50%. [Background technology]

[0002] Plant primary cell walls contain cellulose microfibrils, hemicellulose, and pectin. In native primary cell walls, cellulose microfibrils are connected by hemicellulose and bound to a pectin matrix to form a rigid 2D structure. Primary cell wall material is widely available on an industrial scale, for example, in the form of waste streams from the citrus processing industry. It is known that such primary cell wall material, optionally after depectinization, can be defibrated (also known as activated) by high-shear treatment, such as high-pressure homogenization in the presence of an aqueous medium. In defibrated primary cell wall material, the cellulose fibrils are disentangled and largely reorganized from a 2D structure into a more 3D structure. This results in an increased surface area for the primary cell wall material, providing improved functionality or structure in aqueous media. When used in products as part of the aqueous phase, this allows for improved high temperature (e.g., 45-50°C) stability, suspension of benefit particles (e.g., silicone droplets, anti-dandruff agents, mica or fragrance capsules) and / or foam stability of the product in which they are present.

[0003] The crystallinity of cellulose is characteristic of the source of the material used. For example, bacterial cellulose or wood pulp cellulose (i.e., paper pulp cellulose) has a crystallinity of more than 50%. Cellulose derived from the primary cell walls of non-woody plant parts (e.g., citrus fruit) has a crystallinity of 50% or less.

[0004] It is desirable to provide the defibrated primary cell wall material in a dry form to reduce bulk and energy consumption for transportation. However, once dried, such compositions require high shear treatment again to fully restore their structuring properties in aqueous media. This is undesirable because high shear equipment increases the cost and energy input for manufacturing products using dry defibrated primary cell wall material. Furthermore, this may also limit its applicability to products containing shear-sensitive ingredients. For example, many hair care products contain encapsulated materials, which may be sensitive to high shear treatment.

[0005] US2001 / 0004869A1 describes the use of co-additives homogenized with nanofibrils (microfibrils) to provide a dry composition that can be more easily dispersed in water. In particular, it describes the use of one or more co-additives selected from carboxymethylcellulose with a degree of substitution of up to 0.95, saccharide monomers or oligomers, certain compounds of the formula (R1R2N)COA, and / or cationic or amphoteric surfactants. First, the required use of carboxymethylcellulose is undesirable because it is a chemically modified form of cellulose, which reduces consumer acceptance of products containing it. Second, it has been observed that when using such co-additives, the functionality of the dry cellulose nanofibril composition leaves something to be desired, as incomplete recovery of functional properties has been observed, especially when low-shear mixing is used.

[0006] WO2017 / 019752 discloses citrus fiber in dry form having a storage modulus (G') of at least 50 Pa (said G' is measured on an aqueous medium containing 2% by weight of citrus fiber dispersed therein under low shear agitation of less than 10,000 rpm). The citrus fiber can be included in a composition that includes a surfactant system.

[0007] To be clear, dispersibility in water is not an issue with the dry form of the defibrated primary cell wall material, but rather the restoration of the functional properties imparted to aqueous media by the defibrated cell wall material. This is believed to be due to the fact that when the defibrated material is dried, it forms clumps that are easily dispersible, but which themselves require further disruption and deagglomeration, requiring high shear, to restore the original functional properties.

[0008] It is an object of the present invention to provide a composition comprising dry defibrated primary cell wall material containing cellulose microfibrils, wherein the cellulose has a crystallinity of less than 50%, which is capable of providing improved structuring under low shear mixing in a liquid medium, preferably an aqueous medium.

[0009] Furthermore, in view of improved consumer acceptance of short ingredient lists, it is desirable that the solution contain no additional ingredients beyond those already found in products in which the liquid medium is structured by defibrated primary cell wall material, particularly in the case of household and personal cleaning products used on a regular basis (daily / weekly). [Prior art documents] [Patent documents]

[0010] [Patent Document 1] US2001 / 0004869A1 [Patent Document 2] WO2017 / 019752 Summary of the Invention

[0011] Thus, in a first aspect, the present invention provides a hair cleansing composition comprising: a) 1 to 50 wt. % of a cleansing surfactant selected from the group consisting of anionic surfactants, zwitterionic or amphoteric surfactants, nonionic surfactants, and mixtures thereof; and b) 0.01 to 3% by weight (preferably 0.02 to 2%, more preferably 0.05 to 1.5% by weight) of defibrated primary cell wall material containing cellulose microfibrils, based on the weight of the total composition A composition comprising: the defibrated primary cell wall material contains up to 20% water by weight, based on the total weight of the fibrils; the cellulose has an average crystallinity of less than 50%; A composition is provided in which the defibrated primary cell wall material comprises a polyol distributed between the fibrils.

[0012] In a second aspect of the present invention, there is provided a method of washing comprising applying to hair the hair wash composition of the first aspect.

[0013] In a third aspect, the present invention provides a method for producing a composition according to the first aspect, comprising the steps of: a) providing defibrated primary cell wall material comprising cellulose microfibrils, wherein: the defibrated primary cell wall material contains up to 20% water by weight, based on the total weight of the fibrils; · the cellulose has an average crystallinity of less than 50% and includes a polyol wherein the defibrated primary cell wall material is distributed between the fibrils; b) providing at least an aqueous phase and further ingredients comprising 1 to 50 wt. % of a cleansing surfactant selected from the group consisting of anionic surfactants, zwitterionic or amphoteric surfactants, nonionic surfactants and mixtures thereof; c) mixing the ingredients provided in steps a) and b) under low shear to provide a cleaning product, wherein low shear means using a rotor-stator type mixer or a dispersing disc type mixer having a rotor or disc tip speed of less than 40 m / s, preferably between 5 and 35 m / s, more preferably between 10 and 30 m / s. The present invention provides a method comprising:

[0014] The advantage of this material is that it can be dried with polyol. The resulting dry fibers are then more easily redispersed using relatively low shear, delivering their full structuring potential.

[0015] The polyol distributed among the fibrils improves the recovery of defibrillated fibrils containing up to 20% by weight of water, based on the total weight of the fibrils, when mixed with an aqueous phase. This allows for improved structuring during low-shear mixing with the aqueous phase. This allows the process for producing structured liquid compositions to use low-shear equipment and is therefore much more efficient. DETAILED DESCRIPTION OF THE INVENTION

[0016] Any feature of a particular embodiment of the present invention may be utilized in any other embodiment of the present invention. The word "comprising" is intended to mean "including," but does not necessarily mean "consisting of" or "composed of." In other words, the listed steps or options need not be exhaustive. It should be noted that the examples given in the following description are intended to clarify the present invention and are not intended to limit the present invention to those examples themselves. All weight percentages (wt%) are based on the final weight of the composition unless otherwise indicated. Similarly, all volume percentages (vol%) are based on the final volume of the composition unless otherwise indicated. Except in the examples and comparative experiments, or unless otherwise explicitly indicated, all numbers in this description indicating amounts of materials or reaction conditions, physical properties and / or uses of materials should be understood to be modified by the word "about." Unless otherwise specified, numerical ranges expressed in the form "from x to y" are understood to include x and y. For a particular feature, when multiple preferred ranges are expressed in the format "from x to y," it is understood that all ranges combining the different endpoints are also contemplated. For purposes of this invention, ambient temperature (or room temperature) is defined as a temperature of about 20°C.

[0017] composition Preferably, the defibrated primary cell wall material contains up to 15% by weight water, more preferably up to 12% by weight, even more preferably up to 10% by weight, and even more preferably up to 8% by weight water, based on the total weight of the fibrils.

[0018] Thus, the defibrated primary cell wall material can optionally contain (e.g., encapsulated) water, so long as it remains sufficiently dry. Preferably, the defibrated primary cell wall material of the composition according to the invention contains up to 20% by weight, preferably up to 15% by weight, more preferably up to 12% by weight, even more preferably up to 10% by weight, and even more preferably up to 8% by weight of water, preferably based on the total weight of the fibrils, for example 0.01 to 20% by weight, preferably 0.01 to 15% by weight, more preferably 0.01 to 12% by weight, even more preferably 0.01 to 10% by weight, and even more preferably 0.01 to 8% by weight of water, preferably based on the total weight of the fibrils.

[0019] Primary cell wall material In general, primary cell wall materials typically contain cellulose microfibrils, hemicellulose, pectin, and often lignin. This is in contrast to fungal (composed of chitin) and bacterial (composed of peptidoglycan) cell walls. Primary plant cell walls contain only small amounts, if any, of lignin. Primary cell wall materials according to the present invention may contain some lignin, preferably up to 10% by weight, calculated relative to the total amount of cell wall material, and more preferably do not contain substantial amounts of lignified tissue. Even more preferably, the primary cell wall material consists essentially of non-ligninized tissue, as understood by those skilled in the art of plant biology. Preferably, at least 50% by weight, more preferably at least 75% by weight, and even more preferably 90% by weight of the primary cell wall material is derived from plant parenchyma tissue. The source of plant parenchyma cells may be any plant containing plant parenchyma cells with a cellulose skeleton.

[0020] Preferably, the primary cell wall material comprises primary cell wall material derived from fruits, roots, bulbs, tubers, seeds, leaves, and combinations thereof (preferably the parenchyma thereof), more preferably from citrus fruits, tomato fruits, peach fruits, pumpkin fruits, kiwi fruits, apple fruits, mango fruits, sugar beets, beetroots, turnips, parsnips, corn, oats, wheat, peas, and combinations thereof; even more preferably from citrus fruits, tomato fruits, and combinations thereof. The most preferred source of primary cell wall material is derived from citrus fruits (preferably the parenchyma thereof). The Citrus family is a large and diverse family of flowering plants. Common varieties of citrus fruits include oranges, sweet oranges, clementines, kumquats, tangerines, tangelos, satsuma mandarins, grapefruits, citrons, pomegranates, lemons, rough lemons, limes, and reach limes.

[0021] The primary cell wall material preferably undergoes several pretreatment steps before being defibrated. Such pretreatment preferably includes one or more of the steps of heating, cooking, washing, refining, and depectinization, and more preferably includes the steps of washing and / or depectinization. Preferably, the "primary cell wall material" is primary cell wall material from which most (i.e., more than 50% by weight), preferably essentially all, of all water-soluble components have been removed. Water-soluble components are those that can be removed by washing with water at a temperature of 20°C. Preferably, the source of primary cell wall material is in the form of a washed paste or pulp. Such is commercially available from Herbafood (Citrus fiber AQ+N).

[0022] Plant cell walls, particularly in parenchymal tissues, contain hemicellulose and pectin in addition to cellulose microfibrils. However, the primary cell wall material of the present invention does not need to contain hemicellulose and / or pectin. Hemicellulose may be (partially) removed when the primary cell wall material is prepared / pretreated. Preferably, the primary cell wall material contains up to 40% by weight, more preferably up to 30% by weight, even more preferably up to 20% by weight, and even more preferably up to 5% by weight of hemicellulose, based on the total dry weight of the primary cell wall material. Similarly, pectin may be (partially) removed when the primary cell wall material is prepared / pretreated. Preferably, the primary cell wall material contains up to 30% by weight, more preferably up to 25% by weight, even more preferably up to 20% by weight, and even more preferably up to 5% by weight of pectin, based on the total dry weight of the primary cell wall material.

[0023] cellulose microfibrils Cellulose microfibrils are well known in the art. A typical microfibril generally contains 20 to 50 aligned β-1-4-glucose polymer chains. In natural primary cell wall materials, cellulose microfibrils may be present (partially) in the form of aggregates that make up the cell wall.

[0024] Preferably, the primary cell wall material according to the present invention comprises at least 50% by weight, more preferably at least 60% by weight, even more preferably at least 70% by weight, even more preferably 80% by weight, and even more preferably 90% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material. Even more preferably, the primary cell wall material consists essentially of cellulose microfibrils.

[0025] The weight percentage of cellulose microfibrils in the primary cell wall material is preferably increased by removing soluble and unbound sugars, proteins, polysaccharides, oil-soluble oils, waxes, and phytochemicals (e.g., carotenoids, lycopene). This is suitably accomplished using well-known techniques, including cutting, cooking, washing, centrifuging, decanting, and drying the cell wall material, as is well known to those skilled in the art.

[0026] The compositions of the present invention comprise defibrated cell wall material, i.e., the cellulose microfibrils present in the primary cell walls have been at least partially disentangled, preferably without substantially destroying them. Preferably, the average length of the cellulose microfibrils in the defibrated primary cell wall material is greater than 1 micrometer, preferably greater than 5 micrometers.

[0027] Preferably, at least 80% by weight of the cellulose microfibrils have a diameter smaller than 50 nm, more preferably smaller than 40 nm, even more preferably smaller than 30 nm, even more preferably smaller than 20 nm, and even more preferably smaller than 10 nm. Microfibril diameter is determined using the following method using transmission electron microscopy (TEM) according to (D. Harris et al. Tools for Cellulose Analysis in Plant Cell Walls Plant Physiology, 2010(153),420). Specifically, dispersions of plant sources rich in primary cell wall material are diluted in distilled water to produce thin layers. These dispersions are then imaged on carbon-only 300-mesh copper TEM grids (Agar Scientific) using a Tecnai 20 transmission electron microscope (FEI Company) operating at a voltage of 200 kV. To enhance image contrast between individual microfibrils, a 2% phosphotungstic acid solution at pH 5.2 is used as a negative dye. To do this, the TEM grids with the fibers are incubated in 2% phosphotungstic acid and allowed to air dry after removing excess fluid.

[0028] The cellulose microfibrils according to the invention preferably have an average crystallinity of less than 50%, preferably up to 40%, more preferably up to 35%, even more preferably up to 30% of the cellulose in the microfibrils.

[0029] Table 1 shows the average crystallinity of typical sources of cellulose microfibrils, showing that cellulose in primary cell wall material sourced from plant parenchyma typically has a crystallinity of less than 50% by weight.

[0030] [Table 1]

[0031] The average crystallinity is measured using wide-angle X-ray scattering (WAXS) according to the following protocol and method: Measurements are performed using a Bruker D8 Discover X-ray diffractometer equipped with a GADDS (General Area Detector Diffraction System) (Bruker-AXS, Delft, NL) (Part Number: 882-014900 Serial Number: 02-826) in theta / theta configuration. A copper anode is used, and K-alpha radiation with a wavelength of 0.15418 nm is selected. The instrument parameters used are listed in Table 2.

[0032] [Table 2]

[0033] The average crystallinity (Xc) is calculated by the following formula:

[0034]

number

[0035] Bruker EVA software (version 12.0) is used to separate the regions of the diffraction lines of the crystalline phase from the regions of the amorphous phase.

[0036] Preferably, the fiber is defibrated citrus fiber, free of intact cell walls. Preferred sources from which the defibrated citrus fiber is derived are selected from whole citrus peel, (fully or partially) depectinized citrus peel, or commercially available dried or slurried fiber. Preferred fibers are citrus peel-derived fibers that are 100% self-suspended at 0.3% solids in 0-0.1 L of water at room temperature and have the physical properties of a G' plateau value of 1-5 Pa at 0.3% solids and a G' plateau value of 800-1500 Pa at 1.7% solids.

[0037] In a preferred embodiment, the fiber is an activated citrus fiber having the following characteristics: (i) Self-suspending ability of 45-58% (measured when dispersed at 8000 rpm for 10 minutes at 0.1 wt% dry fiber in the presence of glycerol) (ii) G' is between 600 and 1200 Pa (measured with 2.0 wt. % dry fiber and 10 to 40 wt. % glycerol dispersed in the presence of glycerol at 8000 rpm for 10 min). wherein the measurements (i) and (ii) above are carried out as specified in patent application no. EP15178987.2.

[0038] polyol A polyol is an alcohol containing multiple (i.e., two or more) hydroxyl groups. The polyol may be a monomeric or polymeric polyol. Preferably, the polyol is monomeric.

[0039] For example, sugar alcohols such as sorbitol or sucrose. Preferably, the polyol has a molecular weight of up to 400 MW, more preferably selected from glycerol, diglycerol, monopropylene glycol, dipropylene glycol, ethylene glycol and polyethylene glycol, sorbitol, sucrose and mixtures thereof, most preferably selected from glycerol, sorbitol, sucrose and mixtures thereof. Even more preferred polyethylene glycols are diethylene glycol and triethylene glycol.

[0040] Preferably, the polyol contains 2 to 50, more preferably 2 to 20, even more preferably 2 to 10, even more preferably 2 to 5, and even more preferably 2 hydroxyl groups.

[0041] The polyol is distributed among the fibrils used in the cleaning compositions of the present invention. Additional polyols are also optionally present in the compositions.

[0042] In a preferred embodiment, the polyol distributed among the fibrils used in the present invention is most preferably glycerol, present in an amount of 10 to 40% by weight, based on the weight of the total dry weight of the fibrils.

[0043] In particular, it has been observed that the use of polyols at levels of at least 15% by weight based on the total dry weight of the fibrils provides improved recovery of structuring capacity.

[0044] By "distributed between the fibrils" it is understood that the polyol is in contact with at least a portion of the surface area of ​​the cellulose microfibrils. Surprisingly, it has been observed that the presence of said polyol distributed between the fibrils reduces the energy / shear requirement for defibrated materials containing up to 20 wt. % water, based on the total dry weight of the fibrils, to recover their structuring capacity when mixed with an aqueous medium.

[0045] Preferably, the total amount of polyols in the hair wash composition (including the polyol distributed between the fibers and any additional polyols) is at least 10% by weight, more preferably 15-1000% by weight, even more preferably 20-500% by weight, based on the dry weight of the primary cell wall material in the final composition according to the invention.

[0046] Preferably, the amount of polyol added to the cleaning composition, including polyol resulting from the addition of the composition according to the present invention and additional polyol added directly to the cleaning composition, is at least 0.001 wt. %, preferably 0.0015 wt. % to 10 wt. %, more preferably 0.002 wt. % to 5 wt. % by weight of the total cleaning composition.

[0047] The amount of polyol distributed between the fibrils is suitably present in an amount of 0.001 to 0.05 wt. % by weight of the total composition, and any additional polyol not distributed within the fibrils is suitably present in an amount of 0.15 to 10 wt. %, preferably 0.25 to 5 wt. %, most preferably 0.5 to 3 wt. % by weight of the total composition.

[0048] The polyols according to the invention are preferably water-soluble, which allows for improved distribution between the fibrils and results in improved recovery of the structuring capacity. More preferably, they are water-soluble at a concentration of 0.2% by weight, even more preferably at a concentration of 0.5% by weight, even more preferably at a concentration of 1.0% by weight, and even more preferably at a concentration of 2.0% by weight, measured in (pure) water at ambient conditions.

[0049] Method for producing the composition In step a) of the method for producing a composition according to the invention, primary cell wall material comprising cellulose microfibrils is defibrated by subjecting it to sufficient mechanical energy (e.g., shearing). The source of primary cell wall material is preferably undefibrated, although already defibrated material can be suitably used (and converted into a composition according to the invention comprising a polyol distributed between the fibrils). Undefibrated primary cell wall material itself, without the presence of a polyol distributed between the fibrils, is commercially available, for example, as fruit and vegetable puree, Herbacel AQ Plus citrus fiber (supplied by Herbafoods).

[0050] Suitable defibrillation techniques are known in the art. Defibrillation is preferably carried out using high shear treatment, pressure homogenization, cavitation, explosion, pressure build-up and pressure drop treatment, colloid milling, vigorous mixing, extrusion, ultrasonic treatment, extrusion, grinding, and combinations thereof, more preferably pressure homogenization. Preferred homogenizers include high-pressure homogenizers manufactured by GEA Niro Soavi, Parma, Italy, such as the NS series, or Gaulin and Rannie series homogenizers manufactured by APV Corporation, Everett, Massachusetts, USA. When using a high-pressure homogenizer, the preferred pressure is 500 bar to 2000 bar, more preferably 600 bar to 1000 bar. Preferably, extrusion, grinding, or a combination thereof is used to defibrate primary cell wall material containing cellulose microfibrils at a higher concentration of 5 to 50% by weight.

[0051] The defibration is carried out in the presence of an aqueous medium. Preferably, the aqueous medium comprises at least 50% by weight, more preferably at least 75% by weight, and even more preferably at least 90% by weight of water. The defibration can be carried out as part of a process for obtaining primary cell wall material. The defibration treatment can be achieved by a single treatment or a series of treatments. The amount of aqueous medium in step a) can vary, but is preferably such that a liquid slurry is formed. Preferably, in step a), the amount of aqueous medium is at least 1-fold, preferably at least 5-fold, more preferably 10-500-fold, and even more preferably 20-200-fold the amount of primary cell wall material, the latter being based on dry weight.

[0052] In step b), the water content of the mixture obtained in step a) is reduced. Depending on the other liquids present, the final composition according to the present invention is in the form of a paste, cake or powder, preferably in the form of a cake or powder, more preferably in the form of a powder. It will be understood that the cake can be suitably converted into a powder by suitable milling. Preferably, the powder is a free-flowing powder. The reduction of water in step b) can be carried out using techniques known in the art. Preferably, the amount of water is reduced using evaporation and / or filtration.

[0053] In a preferred method for preparing the composition according to the present invention, after step a) and before step b), the defibrated primary cell wall material in the aqueous medium is contacted with an organic solvent to obtain a precipitate and a liquid phase, followed by separating the precipitate from the liquid phase to obtain a semi-dry cake of defibrated primary cell wall material having a dry matter content of at least 10% by weight based on the mass of the semi-dry cake. The cake can then be further processed as a mixture in step b). This preferred precipitation step further improves the composition's ability to recover and structure aquatic structures.

[0054] Preferably, the polyol is added in step a).

[0055] Preferably, any further ingredients are added after step b), for example for the preparation of an instant cleaning product composition.

[0056] Cleaning product manufacturing method - step a) The present invention further relates to the use of a composition according to the invention for preparing a hair washing composition comprising an aqueous phase, which allows the use of a low shear mixing process.

[0057] Preferably, the amount of the composition according to the present invention added in step a) of the method for producing a cleaning product is 0.01 to 7.5 wt. % based on the dry weight of the defibrated primary cell wall material containing cellulose microfibrils contained in the composition. The amount of defibrated cell wall material is appropriately selected to achieve the desired effect and depends on the overall product format. More preferably, the amount of the composition added is 0.02 to 5 wt. %, and even more preferably 0.05 to 4 wt. %, based on the dry weight of the defibrated primary cell wall material containing cellulose microfibrils contained in the composition.

[0058] Preferably, the total amount of aqueous phase provided in step a) is from 0.5 to 98% by weight, more preferably from 1 to 95% by weight, even more preferably from 2.5 to 90% by weight, based on the total weight of the cleaning product.

[0059] The inclusion level of the composition according to the present invention in the final hair wash composition is 0.01 to 3 wt %, more preferably 0.02 to 2 wt %, even more preferably 0.05 to 1.5 wt % of defibrated primary cell wall material containing cellulose microfibrils, based on the total weight of the hair wash composition.

[0060] The components can be mixed in any order and / or in any part. For example, a first part of the total components can be mixed, followed by the remainder. The mixing in step a) is carried out under low shear.

[0061] As mentioned above, traditionally, to prepare cleaning products with excellent rheological properties, for example, to utilize the properties of citrus fibers, it is necessary to use equipment that can impart high to very high shear forces during the production of the product. Such equipment includes high-pressure homogenizers, microfluidizers, extruders, and ultrasonicators. Such equipment is usually expensive and uses a relatively large amount of energy during operation, and therefore is preferably not used in step a) of the cleaning product production method, and more preferably is not used at all. Therefore, in step a), preferably, one or more high-pressure homogenizers, microfluidizers, extruders, ultrasonicators, or combinations thereof are not used.

[0062] In contrast, the use of compositions and methods according to the present invention allows for the production of cleaning products under low shear with the same or even better rheological properties when compared to the use of prior art defibrated fibers containing up to 20% by weight water (i.e., without polyol distributed between the fibrils) prepared under high shear. In the methods of the present invention, step a) is preferably carried out by mixing the ingredients under what is defined herein as low shear, for example, using a rotor-stator type mixer known in the art (e.g., rotor-stator mixers supplied by IKA, Ystral, and Silverson) or a dispersive disc type mixer (e.g., but not limited to, a Cowles disc mixer, such as one supplied by Fryma), using a rotor or disc tip speed of less than 40 m / s, more preferably 5 to 35 m / s, and even more preferably 10 to 30 m / s. For clarity, mixers capable of high shear can be used at low shear rates in the methods of the present invention.

[0063] In the method of the present invention, other materials can optionally be added before or during the low shear dispersion of the composition according to the present invention.

[0064] Cleaning product manufacturing method - step b) In step b) of the process for making a cleaning product according to the present invention, further ingredients are added and blended until completely dispersed using methods known in the art.

[0065] The wash product according to the present invention is a hair wash product, preferably a hair wash product.

[0066] Further ingredients In step b), additional ingredients can be optionally added.Preferably, the additional ingredients are those typically found in the target cleaning product, which are known to those skilled in the art.The amount of such additional ingredients is based on the final total weight of the cleaning product, unless otherwise specified.

[0067] surfactants The hair wash product according to the present invention comprises a cleansing surfactant. Surfactants are compounds having hydrophilic and hydrophobic moieties that act to reduce the surface tension of the aqueous solution in which they are dissolved. By cleansing surfactant, we mean that the surfactant provides a cleansing agent (i.e., a cleaning effect) to the personal care surface being treated as part of the cleansing, preferably hair washing, process. The hair wash composition according to the present invention generally comprises one or more cleansing surfactants that are cosmetically acceptable and suitable for topical application to hair. The cleansing surfactant can be selected from anionic, nonionic, amphoteric, and zwitterionic compounds and mixtures thereof.

[0068] The total amount of surfactant present is from 1 to 50% by weight, more preferably from 2 to 25% by weight.

[0069] When the composition of the present invention is a hair wash product, the composition preferably comprises 2 to 40%, more preferably 4 to 25%, of total surfactants, based on the total weight of the composition. When a surfactant mixture incorporating both anionic and nonionic surfactants is used, then the ratio of anionic surfactant to nonionic surfactant is preferably 1:1 to 10:1, more preferably 2:1 to 9:1, and most preferably 3:1 to 8:1.

[0070] Hair cleansing composition The composition of the present invention is a hair cleansing composition.

[0071] Preferably, the cleansing surfactant is sodium lauryl sulfate, sodium lauryl ether sulfate (n)EO (where n is 1 to 3), (C 12~13 ) sodium pareth sulfate, ammonium lauryl sulfate, ammonium lauryl ether sulfate (n)EO (where n is 1 to 3), alpha olefin sulfonate (general formula R 1 -CH=CH-SO3 - M + where R 1 is selected from linear or branched alkyl groups having 14 to 16 carbon atoms and mixtures thereof, and M is a solubilizing cation), lauryl taurate, cocoyl taurate, sodium cocoyl isethionate, lauryl ether carboxylic acid, lauryl betaine, cocobetaine, cocamidopropyl betaine, sodium cocoamphoacetate, sodium laurylamphoacetate, lauryl hydroxysultaine, cocohydroxysultaine, laurylaminopropyl hydroxysultaine, cocoaminopropyl hydroxysultaine, and mixtures thereof.

[0072] Preferably, the mixture of any of anionic, nonionic and amphoteric cleansing surfactants has a ratio of first to second surfactant of 1:1 to 10:1, more preferably 2:1 to 9:1, and most preferably 3:1 to 8:1, based on the weight of the cleansing surfactant in the hair wash composition.

[0073] Preferably, the hair wash composition of the present invention comprises from 1 to 50%, preferably from 2 to 40%, more preferably from 4 to 25% total surfactants, based on the total weight of the composition.

[0074] Hair cleansing composition Hair wash compositions of the present invention are generally aqueous, that is, they have water or an aqueous solution or a lyotropic liquid crystalline phase as their major component.

[0075] Suitably, the hair wash composition comprises from 50 to 98% by weight, preferably from 60 to 92% by weight, of water based on the total weight of the composition.

[0076] Hair wash compositions according to the invention generally comprise one or more cleansing surfactants which are cosmetically acceptable and suitable for topical application to the hair, and which may be selected from anionic, nonionic, amphoteric and zwitterionic compounds and mixtures thereof.

[0077] The total amount of cleansing surfactants in the hair wash composition used in the present invention is generally 1 to 50%, preferably 2 to 40%, more preferably 4 to 25%, by total weight of surfactants based on the total weight of the composition.

[0078] Non-limiting examples of cleansing surfactants include anionic cleansing surfactants, such as alkyl sulfates, alkyl ether sulfates, pareth sulfates, alkaryl sulfonates, alkyl olefin sulfonates, N-alkyl sarcosinates, alkyl phosphates, alkyl ether phosphates, acyl amino acid surfactants, alkyl ether carboxylic acids, acyl taurates, acyl glutamates, alkyl glycinates, and their salts, particularly their sodium, magnesium, ammonium, and mono-, di-, and triethanolamine salts. The alkyl and acyl groups in the preceding list generally contain 8 to 18, preferably 10 to 16, carbon atoms and may be unsaturated. The alkyl ether sulfates, alkyl ether phosphates, and alkyl ether carboxylic acids, and their salts, may contain 1 to 20 ethylene oxide or propylene oxide units per molecule.

[0079] Further non-limiting examples of cleansing surfactants include nonionic cleansing surfactants, which have alkylene oxide, usually ethylene oxide, and generally are aliphatic (C8-C9) having 6 to 30 ethylene oxide groups. 18 ) primary or secondary straight or branched chain alcohols. Other representative cleansing surfactants include mono- or di-alkyl alkanolamides (examples include coco mono-ethanolamide and coco mono-isopropanolamide) and alkyl polyglycosides (APGs). Suitable alkyl polyglycosides for use in the present invention are commercially available, such as those materials identified as Plantapon 1200 and Plantapon 2000 from BASF. Other sugar-derived surfactants that can be included in compositions for use in the present invention include, for example, C12-C18 N-methyl glucamides, such as those described in WO 92 06154 and US 5,194,639. 10 -C 18 N-alkyl (C1-C6) polyhydroxy fatty acid amides of C10 -C 18 and N-alkoxy polyhydroxy fatty acid amides such as N-(3-methoxypropyl) glucamide.

[0080] Additional non-limiting examples of cleansing surfactants can include amphoteric or zwitterionic cleansing surfactants, including alkylamine oxides, alkylbetaines, alkylamidopropylbetaines, alkylsulfobetaines (sultaines), alkylglycinates, alkylcarboxyglycinates, alkylamphoacetates, alkylamphopropionates, alkylamphoglycinates, alkylhydroxysultaines, alkylamidopropylhydroxysultaines, acyltaurates, and acylglutamates, where the alkyl and acyl groups have from 8 to 19 carbon atoms.

[0081] Preferably, the cleansing surfactant is sodium lauryl sulfate, sodium lauryl ether sulfate (n)EO (where n is 1 to 3), (C 12~13 ) sodium pareth sulfate, ammonium lauryl sulfate, ammonium lauryl ether sulfate (n)EO (where n is 1 to 3), alpha olefin sulfonate (general formula R 1 -CH=CH-SO3 - M + where R 1 is selected from linear or branched alkyl groups having 14 to 16 carbon atoms and mixtures thereof, and M is a solubilizing cation), lauryl taurate, sodium cocoyl isethionate, lauryl ether carboxylic acid, lauryl betaine, cocobetaine, cocamidopropyl betaine, sodium cocoamphoacetate, sodium laurylamphoacetate, lauryl hydroxysultaine, cocohydroxysultaine, laurylaminopropyl hydroxysultaine, cocoaminopropyl hydroxysultaine, and mixtures thereof.

[0082] Preferably, the mixture of any of anionic, nonionic and amphoteric cleansing surfactants has a ratio of first to second surfactant of 1:1 to 10:1, more preferably 2:1 to 9:1, and most preferably 3:1 to 8:1, based on the weight of the cleansing surfactant in the hair wash composition.

[0083] Preferably, the hair wash composition of the present invention comprises from 1 to 50%, preferably from 2 to 40%, more preferably from 4 to 25% total surfactants, based on the total weight of the composition.

[0084] Aqueous compositions of the present invention preferably have a pH of 3 to <7 (eg 3 to 6.5), preferably 3.5 to <7, more preferably 3.8 to 6.5.

[0085] Optionally, the hair wash compositions used in the present invention may contain additional ingredients, non-limiting examples of which are set out below, to enhance performance and / or consumer acceptability.

[0086] silicone Optionally, the hair wash compositions of the present invention may contain emulsified droplets of a silicone conditioning agent to enhance conditioning performance.

[0087] The emulsifying silicone is preferably selected from the group consisting of polydiorganosiloxanes, silicone gums, amino-functional silicones, and mixtures thereof.

[0088] Suitable silicones include polydiorganosiloxanes, especially polydimethylsiloxanes with CTFA designation of dimethicone.The polydimethylsiloxanes with hydroxyl end groups and CTFA designation of dimethiconol are also suitable for use in the compositions of the present invention (especially shampoos and conditioners).Also suitable for use in the compositions of the present invention are silicone rubbers with a low degree of crosslinking, as described in WO96 / 31188, for example.

[0089] The viscosity of the emulsified silicone itself (not the emulsion or the final hair conditioning composition) is typically at least 10,000 cst at 25°C, with the viscosity of the silicone itself preferably being at least 60,000 cst, most preferably at least 500,000 cst, and ideally at least 1,000,000 cst. Preferably, the viscosity is less than 10 for ease of formulation. 9 Not exceeding cst.

[0090] Emulsified silicones for use in the hair wash compositions of the present invention typically have a D90 silicone droplet size in the composition of less than 30 microns, preferably less than 20 microns, more preferably less than 10 microns, and ideally between 0.01 and 1 micron. Silicone emulsions having an average silicone droplet size (D50) of 0.15 microns are commonly referred to as microemulsions.

[0091] Silicone particle size can be measured by means of laser light scattering techniques, for example using a 2600D Particle Sizer manufactured by Malvern Instruments.

[0092] Examples of suitable preformed emulsions include Xiameter MEM 1785 and Microemulsion DC2-1865 available from Dow Corning. These are emulsions / microemulsions of dimethiconol. Crosslinked silicone rubbers are also available in preemulsified form, which is advantageous for ease of formulation.

[0093] Another preferred class of silicone to be contained in the hair washing composition of the present invention is amino-functional silicone." amino-functional silicone " means the silicone that contains at least one primary, secondary or tertiary amine group, or quaternary ammonium group.The example of suitable amino-functional silicone includes the polysiloxane with CTFA name "amodimethicone".

[0094] Specific examples of amino-functional silicones suitable for use in the present invention are aminosilicone oils DC2-8220, DC2-8166 and DC2-8566 (all available from Dow Corning).

[0095] Suitable quaternary silicone polymers are described in EP-A-0 530 974. A preferred quaternary silicone polymer is K3474 (Goldschmidt).

[0096] Emulsions of amino-functional silicone oils with non-ionic and / or cationic surfactants are also suitable.

[0097] Preformed emulsions of amino-functional silicones are also available from silicone oil suppliers such as Dow Corning and General Electric. Specific examples include DC939 cationic emulsion and nonionic emulsions DC2-7224, DC2-8467, DC2-8177, and DC2-8154 (all from Dow Corning).

[0098] The total amount of silicone is preferably 0.01 to 10% by weight, more preferably 0.1 to 5% by weight, and most preferably 0.5 to 3% by weight of the entire hair wash composition.

[0099] cationic polymer Optionally, the hair wash compositions of the present invention may contain a cationic polymer to enhance conditioning performance.

[0100] Suitable cationic polymers may be cationically substituted homopolymers or may be formed from two or more types of monomers. The weight average (M wThe molecular weight of the polymer is generally between 100,000 and 3,000,000 daltons. The polymer has cationic nitrogen-containing groups, such as quaternary ammonium or protonated amino groups, or a mixture thereof. If the molecular weight of the polymer is too low, the conditioning effect is insufficient. If it is too high, there may be a problem of high extensional viscosity, which can lead to stringiness of the composition when poured.

[0101] Cationic nitrogen-containing groups are generally present as substituents on only a few of the monomer units in a cationic polymer. Therefore, if the polymer is not a homopolymer, it can contain spacer non-cationic monomer units. Such polymers are described in the CTFA Cosmetic Ingredient Directory, Third Edition. The ratio of cationic to non-cationic monomer units is selected to provide a polymer with a cationic charge density in the required range, generally 0.2 to 3.0 meq / gm. The cationic charge density of a polymer is suitably determined via the Kjeldahl method described in the United States Pharmacopeia under Chemical Tests for Nitrogen Determination.

[0102] Suitable cationic polymers include, for example, copolymers of vinyl monomers having cationic amine or quaternary ammonium functionality with water-soluble spacer monomers such as (meth)acrylamides, alkyl and dialkyl (meth)acrylamides, alkyl (meth)acrylates, vinyl caprolactone, and vinyl pyrrolidine. The alkyl and dialkyl-substituted monomers preferably have C1-C7 alkyl groups, more preferably C1-C3 alkyl groups. Other suitable spacers include vinyl esters, vinyl alcohol, maleic anhydride, propylene glycol, and ethylene glycol.

[0103] The cationic amines may be primary, secondary, or tertiary amines, depending on the particular species and the pH of the composition. Generally, secondary and tertiary amines, especially tertiary amines, are preferred.

[0104] Amine-substituted vinyl monomers and amines can be polymerized in the amine form and then converted to ammonium by quaternization.

[0105] The cationic polymer may comprise a mixture of monomer units derived from amine- and / or quaternary ammonium-substituted monomers and / or compatible spacer monomers.

[0106] Suitable (non-limiting examples) cationic polymers include: cationic diallyl quaternary ammonium-containing polymers, such as dimethyldiallylammonium chloride homopolymer and copolymer of acrylamide and dimethyldiallylammonium chloride, referred to in the industry (CTFA) as Polyquaternium 6 and Polyquaternium 7, respectively; mineral acid salts of aminoalkyl esters of homopolymers and copolymers of unsaturated carboxylic acids having 3 to 5 carbon atoms (as described in U.S. Pat. No. 4,009,256); Cationic polyacrylamides (described in WO 95 / 22311).

[0107] Other cationic polymers that can be used include cationic polysaccharide polymers such as cationic cellulose derivatives, cationic starch derivatives, and cationic guar gum derivatives.

[0108] Cationic polysaccharide polymers suitable for use in compositions for use in the present invention include monomers of the formula: AO-[RN + (R 1 )(R 2 )(R 3 )X - ] where A is an anhydroglucose residue, such as a starch or cellulose anhydroglucose residue, and R is an alkylene, oxyalkylene, polyoxyalkylene, or hydroxyalkylene group, or a combination thereof.1 , R 2 and R 3 independently represent an alkyl, aryl, alkylaryl, arylalkyl, alkoxyalkyl, or alkoxyaryl group, each containing up to about 18 carbon atoms. The total number of carbon atoms in each cationic moiety (i.e., R 1 , R 2 and R 3 The total number of carbon atoms in the alkyl group is preferably about 20 or less, and X is an anionic counterion.

[0109] Another type of cationic cellulose includes polymeric quaternary ammonium salts of hydroxyethyl cellulose reacted with lauryldimethylammonium-substituted epoxides, referred to in the industry (CTFA) as Polyquaternium 24. These materials are available from Amerchol Corporation, for example, under the trade name Polymer LM-200.

[0110] Other suitable cationic polysaccharide polymers include quaternary nitrogen-containing cellulose ethers (e.g., as described in U.S. Pat. No. 3,962,418) and copolymers of etherified cellulose and starch (e.g., as described in U.S. Pat. No. 3,958,581). Examples of such materials include the Polymer LR and JR series from Dow, commonly referred to in the industry (CTFA) as Polyquaternium 10.

[0111] A particularly suitable type of cationic polysaccharide polymer that can be used is a cationic guar gum derivative, such as guar hydroxypropyltrimethylammonium chloride (commercially available from Rhodia in their JAGUAR trademark series). Examples of such materials are JAGUAR C13S, JAGUAR C14, and JAGUAR C17.

[0112] Mixtures of any of the above cationic polymers can be used.

[0113] The cationic polymer may be present in hair wash compositions for use in the present invention at a level of from 0.01 to 5%, preferably from 0.02 to 1%, more preferably from 0.05 to 0.8%, by total weight of cationic polymer based on the total weight of the composition.

[0114] Additional ingredients Hair wash compositions for use in the present invention may further comprise additional optional ingredients to enhance performance and / or consumer acceptability, preferably selected from the group consisting of at least one of antimicrobial agents, antidandruff agents, foam boosters, fragrances, encapsulates (e.g., encapsulated fragrances), dyes, colorants, pigments, preservatives, thickeners, proteins, phosphate esters, buffers, pH adjusters, opacifiers, viscosity modifiers, emollients, sunscreens, emulsifiers, sensory actives (e.g., menthol and menthol derivatives), vitamins, mineral oil, essential oils, lipids, natural actives, glycerin, natural hair nutrients such as plant and fruit extracts, sugar derivatives and amino acids, microcrystalline cellulose, and mixtures thereof.

[0115] Preferably, the hair wash composition of the present invention comprises, by weight of the total composition, 0.01 to 20% by weight of an optional ingredient, more preferably 0.05 to 10% by weight, even more preferably 0.075 to 7.5% by weight, and most preferably 0.1 to 5% by weight of at least one cosmetic ingredient.

[0116] When the hair wash composition of the present invention is an anti-dandruff shampoo, it comprises anti-dandruff.

[0117] Antidandruff agents are compounds that are active against dandruff and are typically antibacterial, preferably antifungal, agents. Antidandruff agents typically exhibit a minimum inhibitory concentration of about 50 mg / ml or less against Malassezia.

[0118] The total amount of anti-dandruff agent is preferably present at a level of from 0.01% to 30% by weight of the total hair wash composition, more preferably from 0.05% to 10%, even more preferably from 0.1% to 5%, and most preferably from 0.2% to 4%.

[0119] The anti-dandruff agent is preferably selected from metal pyrithiones, azoles, octopirox (piroctone olamine), selenium sulfide, salicylic acid and combinations thereof, preferably metal pyrithiones, azoles and octopirox, and mixtures thereof.

[0120] Suitable metal pyrithiones include zinc pyrithione, copper pyrithione, silver pyrithione, zirconium pyrithione, and mixtures thereof. The most preferred metal pyrithione is zinc pyrithione.

[0121] When the antidandruff agent is zinc pyrithione, the preferred level in the hair wash compositions of the present invention is 0.1 to 3%, more preferably 0.2 to 2%, and most preferably 0.5 to 1.5%, by weight based on the total weight of the composition. The zinc pyrithione particles may be amorphous or may take on a variety of regular or irregular crystalline forms, such as rods, needles, blocks, platelets, and mixtures thereof. The average particle size (maximum dimension) of the zinc pyrithione particles is typically about 0.1 to about 50 μm, preferably about 0.1 μm to about 10 μm, and more preferably about 0.1 μm to about 5 μm, as measured, for example, using a Horiba LA-910 laser scattering particle size distribution analyzer.

[0122] Azole antifungal agents include ketoconazole and climbazole, with climbazole being preferred.

[0123] Other suitable anti-dandruff agents are octopirox (piroctone olamine), selenium sulfide and salicylic acid.

[0124] suspended particles The compositions of the present invention preferably contain suspended particles, which provide benefits such as visual appearance, fragrance, anti-dandruff, lubrication, etc.

[0125] The suspended particles are preferably selected from silicone droplets, petrolatum, insoluble anti-dandruff agents, appearance modifiers (pearlescent agents) and microcapsules.

[0126] Pearlizing agents can be included to improve the visual appearance and / or consumer appeal of the product. Preferably, the pearlizing agent is selected from mica, titanium dioxide, titanium dioxide-coated mica, glycol distearate, and mixtures thereof.

[0127] The suspended particles may be microcapsules. The benefit agent in the core of the microcapsule may be suitably selected from fragrances, cosmetic active ingredients such as antibacterial agents, antidandruff agents, moisturizers, conditioning agents, sunscreens, physiological cooling agents and emollient oils; and mixtures thereof.

[0128] In the context of the present invention, the term "benefit agent" includes materials that can provide benefit to the hair and / or scalp as well as materials that are beneficially incorporated into personal cleansing compositions, such as cosmetic agents.

[0129] The polymeric shell of the microcapsules may be prepared using methods known to those skilled in the art, such as coacervation, interfacial polymerization and polycondensation.

[0130] The process of coacervation typically involves the encapsulation of a generally water-insoluble material by the precipitation of one or more colloidal materials onto the surface of droplets of that material. Coacervation can be simple, using a single colloid, such as gelatin, or it can involve complexes in which two or sometimes more colloids of opposite charge, such as gelatin and gum arabic or gelatin and carboxymethylcellulose, are used under carefully controlled conditions of pH, temperature, and concentration.

[0131] Interfacial polymerization produces an encapsulation shell from the reaction of at least one oil-soluble wall-forming material present in an oil phase with at least one water-soluble wall-forming material present in an aqueous phase. A polymerization reaction occurs between the two wall-forming materials, forming a covalent bond at the interface between the oil and aqueous phases, forming the capsule wall. An example of a shell capsule produced by this method is a polyurethane capsule.

[0132] Polycondensation involves forming a dispersion or emulsion of a water-insoluble material (e.g., fragrance) in an aqueous solution of a pre-concentrate of polymeric material under appropriate conditions of agitation to produce capsules of the desired size, and adjusting the reaction conditions to cause condensation of the pre-concentrate by acid catalysis, such that the condensate separates from the solution and surrounds the dispersed water-insoluble material, producing a coherent film and the desired microcapsules.

[0133] The preferred method for forming microcapsules for use in the present invention is polycondensation, typically to produce aminoplast encapsulates. Aminoplast resins are the reaction products of one or more amines with one or more aldehydes. Examples of suitable amines include urea, thiourea, melamine and its derivatives, benzoguanamine and acetoguanamine, and combinations of amines.

[0134] Preferably, the polymer shell of the microcapsules is an aminoplast resin selected from melamine formaldehyde, urea formaldehyde, melamine glioxal, and polyureas formed by the reaction of polyisocyanates with polyamines. Most preferred polymer shells are selected from melamine glioxal and polyureas.

[0135] Advantageously, the polymer shell constitutes up to 20% by weight of the microcapsule.

[0136] By varying the process conditions, microcapsules of the desired size can be produced by known methods. The microcapsules typically have an average diameter in the range of 1 to 500 microns, preferably 1 to 300 microns, more preferably 1 to 50 microns, and most preferably 1 to 10 microns. If necessary, the initially produced microcapsules may be filtered or screened to produce a product with greater size uniformity.

[0137] In a typical composition according to the invention, the level of microcapsules (iii) will generally be in the range of 0.2 to 2% by weight, preferably 0.5 to 1.5% by weight, based on the total weight of the composition.

[0138] Fragrance capsules are a preferred type of microcapsule suitable for use in the present invention.

[0139] The hair wash composition is preferably a hair shampoo composition. During use, the composition is typically rinsed off with water.

[0140] The invention is illustrated by the following non-limiting examples. [Example]

[0141] material The materials and compositions used are detailed in Table 3.

[0142] [Table 3]

[0143] Method for producing the composition according to the present invention (Examples 1 and 2) Step (1): Water was added to the depectinized citrus peel to obtain an aqueous slurry with a dry matter content of approximately 4% by weight. The slurry was then fed once into a pressure homogenizer (APV homogenizer, Rannie 15-20.56) at 600 bar to obtain an aqueous slurry containing citrus fiber. Step (2) A precipitation tank was filled with an aqueous isopropanol solution (approximately 82% by weight isopropanol in water). An aqueous slurry containing citrus fiber was pumped into the precipitation tank under agitation using a volumetric pump, forming a precipitate in the form of granules having a size of 5 mm to 50 mm in the tank. The slurry:isopropanol ratio was 1:2. The slurry was mixed by agitation while being added to the tank, and the precipitate was held in the tank for approximately 30 minutes. Step (3) The precipitate was placed in a centrifuge decanter (Flottweg centrifuge) operated at 4000 rpm or higher to separate the liquid phase (i.e., water and isopropanol) from the citrus fibers. Step (4) Steps (2) and (3) were repeated to subject the precipitate to an extraction process to increase the dry matter content. The extraction process was carried out by feeding the precipitate into a screw press. The speed and pressure of the press were adjusted to obtain a semi-dry cake with a dry matter content of about 22% by weight. Step (5) The semi-dried cake was milled using a Lodige FM 300 DMZ mixer for approximately 15-30 minutes to obtain particles with a size in the 1 mm range. The milled semi-dried cake was mixed with commercially available glycerol at a glycerol:fiber ratio of 1:4 (Example 1) and 1:2.5 (Example 2). Step (6) The ground cake was dried in a ventilated oven at 40°C for about 2 hours to reach a moisture content of about 8% by weight.

[0144] Methods for compositions not according to the invention (Examples 3 and 4) Compositions were prepared according to Example 2, except that sucrose or sorbitol was used instead of glycerol in step 5. Specifically, in Example 3, sucrose was used at a sucrose:fiber ratio of 1:2.5. In Example 4, sorbitol was used at a sorbitol:fiber ratio of 1:2.5.

[0145] Method for manufacturing hair cleansing products Hair wash products were prepared having the formulations shown in Table 4. The process used to prepare the hair wash products is further described below.

[0146] [Table 4]

[0147] Regarding hair cleansing products A1 and B1-B4: As a first step, a coarse premix of the composition (according to Examples 1, 2, 3, 4 or Comparative Example A) and water was prepared, containing a total of 10% by weight of the product formulation (a portion of the water phase was used for this purpose). The premix was stirred for 15 minutes using a paddle mixer operated at 200 rpm to ensure that no clumping occurred.

[0148] The remaining available water in the product was charged to a 50-liter process vessel, and the coarse premix of the composition and water was injected in-line at a rate of 15 kg / hr into the process vessel's recirculation loop immediately upstream of a 150 / 250 Silverson rotor-stator mill operating at a tip speed of 24 m / s. The mixture was continuously recirculated through the Silverson rotor-stator mill at a flow rate of 250 kg / hr for 60 minutes. The mill was then turned off, and the remaining ingredients were added using standard addition methods known in the art to produce a product with a viscosity specification of 4000-6000 cP (RV5, 20 rpm, 30°C, 1 minute) and a pH specification of 5.5-6.5.

[0149] About Hair Cleansing Product C1: Water was added to the depectinized citrus peel to obtain an aqueous slurry with a dry matter content of approximately 2% by weight. The slurry was fed once into a pressure homogenizer (APV homogenizer, Rannie 15-20.56) at 500 bar. An aqueous slurry containing citrus fiber was obtained. The remaining available water in the product was charged into a 50-liter process vessel, and the 2% aqueous slurry was injected in-line at a rate of 15 kg / hr into the process vessel's recirculation loop immediately upstream of a 150 / 250 Silverson rotor-stator mill operating at a tip speed of 24 m / s. The mixture was continuously recirculated through the Silverson rotor-stator mill for 60 minutes at a flow rate of 250 kg / hr. The mill was then turned off and the remaining ingredients were added by standard addition methods known in the art to produce a product with a viscosity specification of 4000-6000 cP (RV5, 20 rpm, 30°C, 1 minute) and a pH specification of 5.5-6.5.

[0150] Shear profile analysis of hair cleansing products A rheological flow curve was then generated for the final hair wash product using the following two-step protocol.

[0151] The instrument used was a Thermo Scientific RS1 (Rheostress 1) with a Z20 DIN, profiled DIN concentric cylinder geometry. Measurements were performed at two temperatures: 25°C and 50°C.

[0152] Step 1 - Controlled stress steps from 0.01 to 400 Pa; 40 logarithmically spaced steps of stress; 0.1 s, spending 40 s at each point to measure shear rate (and therefore viscosity) -1 When the shear rate reaches 100%, step 1 is completed. Step 2 - 0.1~1200s -1 controlled shear rate steps of 40 logarithmically spaced steps of shear rate, spending 6 seconds at each point to determine the shear rate and therefore the stress required to maintain viscosity.

[0153] The results of the first two steps are carefully combined to remove any overlap and ensure that the required shear rate is achieved at the start of the step.

[0154] The yield stress in Pascals (Pa) was then calculated as -1 The stress value at a shear rate of 100 s is taken as the equivalent of the y-axis intercept in a Harschel-Buckley plot of shear stress versus shear rate. The results are shown in Table 5.

[0155] [Table 5]

[0156] When the same low shear process is used to produce hair wash products, the measured yield stress of the hair wash products containing the compositions of the present invention (B1-B4) is greater than that of the hair wash product prepared using Comparative Example A (A1).

[0157] Hair wash products prepared under low shear using compositions (B1-B4) according to the present invention have yield stress measurements comparable to hair wash product (C1) with Comparative Example A, in which high energy treatment in a high pressure homogenizer was used. This highlights the advantage delivered by compositions according to the present invention in enabling the use of low shear processes to deliver hair wash products with higher yield stresses.

[0158] A higher yield stress of the hair wash product gives it greater suspension capacity, which is presumed to result in improved stability of the hair wash product.

Claims

1. A hair cleansing composition comprising: a) 1 to 50 wt. % of a cleansing surfactant selected from the group consisting of anionic surfactants, zwitterionic or amphoteric surfactants, nonionics, and mixtures thereof; and b) 0.01 to 3% by weight of the total composition of defibrated primary cell wall material containing cellulose microfibrils A composition comprising: the defibrated primary cell wall material comprises 0.01 to 20 wt. % water, based on the total weight of the fibrils; the cellulose has an average crystallinity of less than 50%; the defibrated primary cell wall material comprises a polyol distributed between fibrils; the primary cell wall material comprises at least 50% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material; the polyol is water-soluble, The composition, wherein the polyol is selected from glycerol, sorbitol, and sucrose.

2. 10. The composition of claim 1, wherein the defibrated primary cell wall material contains up to 15% water by weight, based on the total weight of the fibrils.

3. 3. The composition of claim 2, wherein the defibrated primary cell wall material contains up to 12% by weight of water, based on the total weight of the fibrils.

4. 3. The composition of claim 2, wherein the defibrated primary cell wall material contains up to 10% by weight of water, based on the total weight of the fibrils.

5. 3. The composition of claim 2, wherein the defibrated primary cell wall material contains up to 8% by weight of water, based on the total weight of the fibrils.

6. The composition according to any one of claims 1 to 5, wherein the composition is a hair shampoo.

7. 10. The composition of claim 1, wherein the primary cell wall material comprises at least 60% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material.

8. 10. The composition of claim 1, wherein the primary cell wall material comprises at least 70% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material.

9. 10. The composition of claim 1, wherein the primary cell wall material comprises at least 80% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material.

10. 10. The composition of claim 1, wherein the primary cell wall material comprises at least 90% by weight of cellulose microfibrils, based on the total dry weight of the primary cell wall material.

11. The composition according to any one of claims 1 to 10, wherein the cellulose microfibrils have an average crystallinity of up to 40%.

12. 12. The composition of claim 11, wherein the cellulose microfibrils have an average crystallinity of up to 35%.

13. 12. The composition of claim 11, wherein the cellulose microfibrils have an average crystallinity of up to 30%.

14. 14. A composition according to any one of claims 1 to 13, wherein the total amount of polyol, including the polyol distributed between the fibres and any optional additional polyol, in the hair wash composition is at least 10 wt.-%, based on the dry weight of the primary cell wall material in the final composition according to the invention.

15. 15. The composition of claim 14, wherein the total amount of polyol, including the polyol distributed between the fibers and any optional additional polyol, in the hair wash composition is from 15 to 1000 wt. %, based on the dry weight of the primary cell wall material in the final composition according to the invention.

16. 15. The composition of claim 14, wherein the total amount of polyol, including the polyol distributed between the fibers and any optional additional polyol, in the hair wash composition is from 20 to 500 wt. %, based on the dry weight of the primary cell wall material in the final composition according to the invention.

17. 17. The composition of any one of claims 1 to 16, wherein the defibrated primary cell wall material comprising cellulose microfibrils is present in an amount of 0.02 to 2 wt. % by weight of the total composition.

18. 18. The composition of claim 17, wherein the defibrated primary cell wall material comprising cellulose microfibrils is present in an amount of 0.05 to 1.5 wt. % by weight of the total composition.

19. The composition of any one of claims 1 to 18, wherein the microfibrils are citrus fibers.

20. 20. The composition of any one of claims 1 to 19, wherein the fiber is an activated citrus fiber having a self-suspending ability of 45-58% (measured on 0.1 wt% dry fiber when dispersed in the presence of glycerol at 8000 rpm for 10 minutes) and a G' of between 600 and 1200 Pa (measured on 2.0 wt% dry fiber and 10-40 wt% glycerol dispersed in the presence of glycerol at 8000 rpm for 10 minutes).

21. A composition according to any preceding claim, wherein the polyol is glycerol present in an amount of 10 to 40% by weight, based on the weight of dry fibre.

22. A method for washing hair, comprising the step of applying to hair a hair wash composition according to any one of claims 1 to 21.

23. A method for producing the hair wash composition according to any one of claims 1 to 21, comprising: a) providing defibrated primary cell wall material comprising cellulose microfibrils, wherein: the defibrated primary cell wall material comprises 0.01 to 20% by weight of water, based on the total weight of the fibrils; the cellulose has an average crystallinity of less than 50%, and wherein the defibrated primary cell wall material comprises a polyol distributed between fibrils, the polyol being water soluble; b) providing further ingredients comprising at least an aqueous phase and 1 to 50 wt. % of a cleansing surfactant selected from the group consisting of anionic surfactants, zwitterionic or amphoteric surfactants, nonionic surfactants and mixtures thereof; c) mixing the ingredients provided in steps a) and b) under low shear to provide a cleaning product, wherein low shear means using a rotor-stator type mixer or a dispersing disc type mixer having a rotor or disc tip speed of less than 40 m / s. A method comprising:

24. 24. The method of claim 23, wherein said low shear means using a rotor-stator type mixer or a dispersion disc type mixer with a rotor or disc tip speed of 5 to 35 m / s.

25. 24. The method of claim 23, wherein said low shear means using a rotor-stator type mixer or a dispersion disc type mixer with a rotor or disc tip speed of 10 to 30 m / s.

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