Unit dose composition, method of making the unit dose composition as a monolithic solid

Abstract

A unit dose composition is provided that allows for the delivery of cleaning materials in a unit dose format that does not require a surrounding film, yet exhibits the necessary hardness and deformation characteristics to maintain product integrity during storage and transport. The present disclosure also provides a method for preparing the unit dose composition configured as a monolithic solid.

Description

[Technical Field]

[0001] The present disclosure relates to a unit dose composition useful for providing various materials, such as cleaning agents, in a unit dosage form. More specifically, the unit dose composition effectively provides various materials in a format that is not partially or completely wrapped or does not need to be wrapped in a material, such as a film or envelope made of poly(vinyl alcohol) (PVOH). The present disclosure also relates to a method for making the unit dose composition. [Background technology]

[0002] There is a growing emphasis on consumer products that are convenient for consumers and less harmful to the environment by, for example, minimizing carbon dioxide emissions through reduced packaging. One example is the emergence of "unit-dose" or "single-dose" systems for laundry applications, dishwashing, and similar uses, in which the essential components are contained in a compact pod or other unit that can be placed in a washing machine, dishwasher, etc. Upon contact with water, the pod or unit is intended to completely dissolve, releasing the cleaning agent ingredients. Such unit-dose systems require less packaging material, are easier to transport (e.g., reduced moisture content or complete removal of moisture), and therefore require lower energy inputs for product distribution.

[0003] Unit dose systems are frequently packaged with the dosage composition contained within an envelope, packaging film, or the like, to compartmentalize the liquid or solid effective amount as individual unit doses (i.e., "pods"). These unit dose systems mostly use poly(vinyl alcohol) (PVOH) as the packaging substrate due to its water solubility. Partially hydrolyzed PVOH, particularly those with a degree of hydrolysis less than 89%, is the most common packaging material of choice due to its higher water solubility compared to more highly hydrolyzed forms. However, PVOH can undergo hydrolysis, especially when in contact with alkaline formulation ingredients commonly present in many cleaning products. As a result, PVOH components, such as pod films, undergo hydrolysis and are converted into poorly water-soluble packaging materials. The poor water solubility can result in ineffective release during cleaning or can leave remnants of the packaging material as residue on the items being washed (e.g., clothing, dishware, etc.). Thus, there remains a need to provide a variety of compositions in convenient unit dosage forms that are stable during shipping and storage, do not require being partially or completely enclosed in a film or envelope, and exhibit high potency while maintaining a unified solid format. Summary of the Invention [Means for solving the problem]

[0004] The present disclosure provides a unit dose composition. More specifically, the unit dose composition can be configured as a monolithic solid that dissolves in water. The composition is a self-supporting unit dose that does not necessarily require an envelope, film, or other type of enclosing layer or component to maintain its shape and mass (i.e., is not acted upon by excessive external force). Also disclosed herein is a method for making a monolithic solid unit dose composition that is not enclosed in a film or envelope.

[0005] In some embodiments, a unit dose composition according to the present disclosure can include an alcohol and anhydrous salt complex, a structuring agent, and a detergent, wherein the unit dose composition is configured as a monolithic solid. In one or more further embodiments, the unit dose composition can be defined in terms of one or more of the following statements, which can be combined in any number or order without departing from the language set forth in the present disclosure:

[0006] The alcohol may be present in an amount of about 30% to about 45% based on the total weight of the unit dose composition. The anhydrous salt may be an anhydrous chloride salt. The anhydrous salt may include a cation having a Pauling electronegativity of at least 1.0. The anhydrous salt may be present in an amount of about 30% to about 45% by weight based on the total weight of the unit dose composition. The structuring agent may comprise a polymer. The structuring agent may include an acetate polymer. The structuring agent may comprise a copolymer of acetate monomer and one or more additional monomers. The structuring agent may be present in an amount of about 5% to about 20% by weight based on the total weight of the unit dose composition.

[0007] The unit dose composition may further comprise a plasticizer. The plasticizer may be a liquid that is effective to partially solubilize the structurant and increase the bonding between the structurant and the alcohol and anhydrous salt complex. The plasticizer may include glycol hexyl ether. The plasticizer may be present in an amount of about 0.1% to about 5% by weight based on the total weight of the unit dose composition. The cleaning agent may be selected from the group consisting of surfactants, builders, alkalizing agents, enzymes, optical brighteners, anti-redeposition polymers, optical brighteners, bleaching agents, pearlescent agents, and combinations thereof.

[0008] The unit dose composition as a monolithic solid can have a hardness value defined by exhibiting a peak force at break of at least 190 Newtons and a percent deformation at peak force of about 20% to about 30% as measured with a Brookfield Texture Analyzer. A unit dose composition as a monolithic solid can be neither partially nor completely enclosed in a film or envelope. The unit dose composition as a monolithic solid may be water soluble. The unit dose composition as a monolithic solid can be configured to achieve at least 95% dissolution in deionized water in a time period of from about 30 seconds to about 8 minutes.

[0009] In some embodiments, a method of making a unit dose composition according to the present disclosure may include combining a structuring agent, a detergent, and an alcohol to form a mixture; combining the mixture with an anhydrous salt to form an intermediate composition; and solidifying the unit dose amount of the intermediate composition under conditions where the anhydrous salt reacts with the alcohol to form a complex that structurally comprises the structuring agent and the detergent to obtain the unit dose amount as a discrete unit of a cohesive solid. The combining may further include combining a plasticizer to form the mixture. [Brief explanation of the drawings]

[0010] [Figure 1] FIG. 1 is a graph showing peak force (hardness) values ​​plotted against the ratio of structurant to anhydrous salt for unit dose compositions prepared as monolithic solids in accordance with embodiments of the present disclosure. [Figure 2] FIG. 2 is a graph showing percent deformation at peak force (hardness) values ​​plotted against the ratio of structurant to anhydrous salt for unit dose compositions prepared as monolithic solids in accordance with embodiments of the present disclosure. [Figure 3] FIG. 3 is a graph showing peak force (hardness) values ​​plotted against the weight percent of plasticizer used in unit dose compositions prepared as monolithic solids according to embodiments of the present disclosure. [Figure 4] FIG. 4 is a graph showing percent deformation at peak force (hardness) values ​​plotted against weight percent of plasticizer used in unit dose compositions prepared as monolithic solids according to embodiments of the present disclosure. DETAILED DESCRIPTION OF THE INVENTION

[0011] The present disclosure is described in more detail below. This disclosure may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will satisfy applicable legal requirements. Like numbers refer to like elements throughout the specification. As used in this specification and claims, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise.

[0012] In one or more embodiments, the present disclosure relates to unit dose compositions configured as a monolithic solid. Configuration as a monolithic solid may refer to the unit dose being a monolithic structure. Preferably, the unit dose is monolithic such that no film or envelope is required to contain the composition within the unit dose. In various embodiments, the unit dose compositions of the present disclosure may include a matrix that is a complex of alcohol and anhydrous salt, carrying and / or incorporating at least the structuring agent and cleaning agent, the matrix defining the monolithic solid structure. Methods of making unit dose compositions as a monolithic solid are also disclosed. Advantageously, configuration as a monolithic solid allows for delivery of cleaning agent ingredients in pre-measured amounts to the location where cleaning power is desired (e.g., washing machine, dishwasher, etc.) without the need for packaging films, envelopes, etc. Rather, the various components are held together by the matrix structure of the alcohol / anhydrous salt complex, such that under normal handling conditions, the unit dose composition substantially retains its original shape and mass as originally manufactured. Normal handling conditions are understood to mean that the unit dose composition remains substantially dry (except under ambient humidity conditions) and is not subjected to excessive force during shipping, storage, and handling. In other words, the unit dose composition exhibits structural integrity not expected of a liquid or powder composition, which may require some type of packaging to maintain the unit dose format.

[0013] In one or more embodiments, the unit dose composition of the present disclosure may comprise a complex of an alcohol and an anhydrous salt. Without wishing to be bound by theory, the alcohol and the anhydrous salt are combined in an exothermic reaction to form an alcoholate, which structurally represents a complex and / or, more specifically, in some embodiments, a crystalline lattice. Thus, in one or more embodiments, the unit dose composition of the present disclosure may be characterized as a complex, matrix, alcoholate, or alcoholate salt, in which the additional components of the unit dose composition are supported or incorporated into the structure defined by the reaction product of the alcohol and the anhydrous salt.

[0014] Various alcohols can be used in the unit dose compositions described herein. The alcohol can be any material having an alcohol functional group. Furthermore, the alcohol is liquid at the alcoholate matrix formulation temperature so that the unit dose composition, which may include one or more of a polymer, a plasticizer, a nonionic surfactant, and a fragrance, can be dissolved or easily dispersed. The alcohol is preferably configured to react effectively with the anhydrous salt component to form the matrix structure as described above. In some embodiments, the alcohol can be a primary alcohol, a secondary alcohol, and / or a tertiary alcohol. A single alcohol can be used, or a mixture of alcohols can be used. Isopropyl alcohol (i.e., propan-2-ol or 2-propanol) is a non-limiting example of an alcohol suitable for forming the matrices described herein. For example, when forming a matrix at 25 degrees Celsius (°C), alcohols ranging from methanol (C1) to 1-decanol (C10), or their isomers, can be used. In some embodiments, any isomer of a higher carbon number alcohol can be used, provided that the alcohol is liquid at the formulation temperature. In certain embodiments, the alcohol may be present in the final unit dose composition in an amount of about 25% to about 55% by weight, about 30% to about 45% by weight, about 32% to about 45% by weight, or about 35% to about 40% by weight, based on the total weight of the unit dose composition. In further embodiments, the unit dose composition may contain at least 20%, at least 25%, at least 30%, or at least 35% by weight of alcohol, based on the total weight of the unit dose composition. In such embodiments, an upper limit (i.e., less than or equal to) may apply, for example, an upper limit of 60%, 55%, 50%, or 45% by weight, based on the total weight of the unit dose composition.

[0015] The anhydrous salt used in the present compositions can be any salt that reacts effectively with alcohol to form an alcoholate matrix. While metal salts are preferred, other salts that react effectively with alcohol to form an alcoholate matrix can be used. In some embodiments, the anhydrous salt can be a Group VII salt, such as a chloride, fluoride, or bromide salt. In further embodiments, the anhydrous salt can be characterized in relation to its cation component. In particular, cations with a higher binding affinity to alcohol can provide stronger intermolecular interactions between the anhydrous salt and the alcohol component of the matrix. The cations of the anhydrous salt can be selected from Group I and Group II metals, with cations with higher electronegativity being preferred. In some embodiments, the anhydrous salt can specifically include cations with an electronegativity of at least 0.98, at least 1.0, or at least 1.2. As such, calcium and magnesium salts are particularly preferred. In particular, anhydrous chloride salts, such as anhydrous calcium chloride and / or anhydrous magnesium chloride, can be particularly useful.

[0016] In various embodiments, the anhydrous salt may be present in the final unit dose composition in an amount of about 15% to about 55%, about 25% to about 50%, about 30% to about 45%, or about 35% to about 45% by weight, based on the total weight of the unit dose composition. In further embodiments, the unit dose composition may contain at least 15%, at least 20%, at least 25%, at least 30%, or at least 35% by weight of the anhydrous salt, based on the total weight of the unit dose composition. In such embodiments, an upper limit (i.e., less than or equal to) may apply, for example, an upper limit of 65%, 60%, 55%, or 50% by weight, based on the total weight of the unit dose composition.

[0017] In some embodiments, compositions can be defined in terms of the ratio of alcohol to salt used to form the composition. In particular, this ratio can be adjusted to define a specific dissolution time of the final unit dose composition in water. The ratio of alcohol to salt can be, for example, about 0.5 to about 5, about 0.8 to about 4, about 0.9 to about 3, or about 1 to about 2, based on the w / w ratio of alcohol concentration to salt concentration. Using a ratio at the higher end of the preferred range can be useful for achieving faster dissolution times in water, and using a ratio at the lower end of the preferred range can be useful for achieving slower dissolution times in water.

[0018] The unit dose compositions of the present disclosure can exhibit improved properties by including one or more ingredients effective to increase the structural integrity of the unit dose composition. A preferred additive may be effective to improve the bonding within the matrix between structures resulting from alcoholate formation. Thus, in one or more embodiments, the unit dose composition may include one or more structuring agents. In one or more embodiments, the structuring agent may be a polymer. Polymers or other structuring agents may be beneficial for providing increased structural integrity to the unit dose composition by improving bonding within the complex. Structuring agents may also be particularly useful for imparting a desired hardness and limiting brittleness. More specifically, the inclusion of a polymeric structuring agent within the alcoholate complex can impart elasticity and / or plasticity, imparting toughness to the unit dose structure while maintaining overall hardness. For example, vinyl acetate polymers or copolymers of vinyl acetate monomer and at least a second monomer can be used. Similarly, vinylpyrrolidone polymers or copolymers of vinylpyrrolidone monomer and at least a second monomer can be used. In a specific embodiment, polyvinylpyrrolidone-co-vinyl acetate (PVAc-PVP) can be used. In some embodiments, povidone polymers can be used, such as povidone sold under the trade name Plasdone (TM).Although such polymers are useful, it is understood that the polymer can generally be any polymer that is soluble in the alcohol used in forming the complex with anhydrous salt.The solubility of polymers in alcohol can be evaluated using the solubility parameter theory, also known as the Hansen solubility parameter, which is a well-known standard for assessing the compatibility of polymers with solvents, where the solubility parameter δ is the square root of the cohesive energy density between solvent molecules and solute (polymer) molecules.This has been described, in particular, by Butreddy et al. [A. Butreddy, S. Sarabu, S. Bandari, A. Batra, K. Lawai, N. Ningyi Chen, V. Bi, T. During, and M.A. Repka, "Influence of Plasdone S630 Ultra - an Improved Copovidone on the Processability and Oxidative Degradation of Quetiapine Fumarate Amorphous Solid Dispersions Prepared via Hot-Melt Extrusion Technique," PharmSci Tech 22, 196 (2021)]. Solubility parameters for various materials can be found in the literature, and in particular for polymers, in various online databases. Otherwise, the solubility parameter can be calculated using the dispersion power (δ). d ), polar force (δ p ), and the forces associated with hydrogen bonds (δ h The solubility parameter can be calculated as a measure of the intermolecular interactions associated with the solubility parameter (solubility parameter). The solubility parameter can be determined by a number of experimental methods cited in the scientific literature. For example, the solubility parameter can be calculated using the Van Krevelen and Hoftyzer group contribution method by using the equation shown below:

[0019]

number

[0020] In the above equation, is the total solubility parameter and δ d , δ p and δ h are parameters related to dispersion forces, polar forces, and hydrogen bonds, respectively, and F di , F pi and E hiare the molar attraction constants due to the dispersion, polar component, and hydrogen bond energy, respectively. V is the molar volume. In addition to the above, solubility parameters can be calculated by group contribution methods such as those by van Krevelen [DW van Krevelen, Fuel 44, 229 (1965)] and van Krevelen and Hoftyzer [DW van Krevelen and PJ Hoftyzer, J. Appl. Polym. Sci. 11, 2189 (1967)]. These methods calculate the (dispersion, polar, or H-bond) solubility parameter δ i (EA Grulke, Polymer Handbook, 3rd ed., J. Bandrup and EH Immergut (Ed.), Wiley, New York, 1989, p.524):

[0021]

number

[0022] (In the formula, Δe j is the evaporation energy contribution associated with functional group j, and n j is the amount of type j groups in the molecule, and V i is the molar volume of species i).

[0023] Without wishing to be bound by theory, one condition for solubility is that the difference in δ between the solvent and the solute is 7 (megapascals). 1 / 2 (MPa) 1 / 2 For example, δ for the polymer Plasdone S630 copolymer is 26.4 (MPa) 1 / 2 and δ for the alcohol isopropanol is 23.5 (MPa) 1 / 2 Therefore, the difference in δ is 2.9 (MPa) 1 / 2 , and it is clearly 7 (MPa) 1 / 2For polymers such as polyacrylate, polyvinylpyrrolidone, polyvinyl acetate, and polyethylene oxide, the absolute value of the corresponding difference in δ is less than 7 (MPa). 1 / 2 In some embodiments, the structuring agent can be used when a solvent is used that has a solubility parameter difference compared to the solvent of less than about 1 (MPa) 1 / 2 to approximately 6.9 (MPa) 1 / 2 , approximately 1.5 (MPa) 1 / 2 to approximately 6.8 (MPa) 1 / 2 , or about 2 (MPa) 1 / 2 to approximately 6.5 (MPa) 1 / 2 In a further embodiment, the difference in solubility parameters may be within the range of 7 (MPa) 1 / 2 Less than 6.8 (MPa) 1 / 2 Less than 6.5 (MPa) 1 / 2 Less than 6 (MPa) 1 / 2 Less than or 5.5 (MPa) 1 / 2 It may be less than.

[0024] In certain embodiments, the structuring agent may be present in the final unit dose structure in an amount of about 5% to about 25%, about 10% to about 22%, or about 12% to about 20% by weight, based on the total weight of the unit dose composition. In further embodiments, the unit dose composition may contain at least 5%, at least 7%, at least 10%, or at least 12% by weight of structuring agent, based on the total weight of the unit dose composition. In such embodiments, an upper limit (i.e., less than or equal to) may apply, for example, an upper limit of 40%, 35%, or 30% by weight, based on the total weight of the unit dose composition.

[0025] In certain embodiments, the physical properties of the unit dose composition may depend, at least in part, on the ratio of the concentration of structuring agent to the concentration of anhydrous salt in the unit dose composition. A particularly appropriate ratio can provide a balance of hardness and resilience that allows the unit dose composition to maintain its unit dose structure by resisting collapse or breakage and by resisting excessive deformation from its original shape. In some embodiments, the ratio of structuring agent to anhydrous salt (wt. / wt.) in the final unit dose composition can range from about 0.1 to about 0.6, from about 0.1 to about 0.5, or from about 0.2 to about 0.5.

[0026] In one or more embodiments, the unit dose composition may include a cleaning agent. As used herein, a cleaning agent may be any material recognized for use in cleaning compositions to provide cleaning efficacy. Cleaning efficacy may be specifically related to clothing or textiles in general. Similarly, cleaning efficacy may be related to dishware or cookware. Additionally, efficacy may be related to industrial applications. Cleaning efficacy may be defined in terms of the ability to at least partially remove soiling materials (e.g., dirt), grease, oil, vegetable stains, etc., that may be present on the item being cleaned. Cleaning efficacy may also be defined in terms of the ability to whiten and / or brighten the item being cleaned. In various embodiments, the cleaning agent may be selected from the group consisting of surfactants, builders, alkalizing agents, enzymes, optical brighteners, anti-redeposition polymers, optical brighteners, bleaching agents, pearlescent agents, and combinations thereof. In various embodiments, the cleaning composition can be any of the following, which are provided non-limitingly and only as examples of types of combinations that may be suitable: one or more nonionic surfactants, one or more anionic surfactants, combinations of one or more nonionic surfactants with one or more anionic surfactants, one or more builders, combinations of one or more builders with one or more nonionic surfactants and / or one or more anionic surfactants, one or more enzymes, combinations of one or more enzymes with one or more nonionic surfactants and / or one or more anionic surfactants and / or one or more builders, one or more bleaching agents, combinations of one or more bleaching agents with one or more nonionic surfactants and / or one or more anionic surfactants and / or one or more builders, combinations of one or more anti-redeposition polymers with one or more nonionic surfactants and / or one or more anionic surfactants and / or one or more builders.

[0027] In various embodiments, suitable anionic surfactants include one or more salts of anionic sulfates, sulfonates, carboxylates, and sarcosinates (e.g., sodium, potassium, ammonium, and substituted ammonium salts, such as mono-, di-, and triethanolamine salts). Exemplary anionic sulfates include linear and / or branched primary and secondary alkyl sulfates, alkyl ethoxy sulfates, fatty acid oleoylglycerol sulfates, alkylphenol ethylene oxide ether sulfates, C5-C6 alkyl esters, C6 alkyl esters, C7 alkyl esters, C8 alkyl esters, C9 alkyl esters, C10 alkyl esters, C11 alkyl esters, C12 alkyl esters, C13 alkyl esters, C14 alkyl esters, C15 alkyl esters, C16 alkyl esters, C17 alkyl esters, C18 alkyl esters, C19 alkyl esters, C18 alkyl esters, C19 alkyl 17 Included are acyl-N-(C1-C4 alkyl) and -N-(C1-C2 hydroxyalkyl) glucamine sulfates, as well as sulfates of alkyl polysaccharides, such as alkyl polyglucoside sulfates. Exemplary alkyl sulfates include linear and / or branched primary C 10 -C 18 Exemplary alkyl ethoxy sulfate surfactants include C alkyl ethoxylates ethoxylated with 0.5 to 20 moles of ethylene oxide per molecule. 10 -C 18 Exemplary anionic sulfonate surfactants include C5-C alkyl sulfates. 20 Linear Alkyl Benzene Sulfonate, Alkyl Ester Sulfonate, C6-C 22 Primary or secondary alkanesulfonates, C6-C 24 Examples of suitable anionic surfactants include olefin sulfonates, sulfonated polycarboxylic acids, alkyl glycerol sulfonates, fatty acid acyl glycerol sulfonates, salts of fatty acid oleyl glycerol sulfonates, and any mixtures thereof. Exemplary anionic carboxylates include alkyl ethoxy carboxylates and alkyl polyethoxy polycarboxylates. In some embodiments, preferred anionic surfactants include various sulfates (e.g., alkyl ether sulfates, e.g., laureth sulfate salts), alkyl ester sulfonates, and alkyl benzene sulfonates (e.g., C5 to C6). 20 or C10 Non-limiting examples of anionic surfactants that can be used in the present invention include sodium laureth sulfate (SLES), sodium lauryl sulfate (SLS), methyl ester sulfonate (MES), and C 10-16 Examples include sodium alkylbenzene sulfonate (LAS). In some embodiments, ethoxylated anionic surfactants can be used, which can contain a limited number of moles of ethylene oxide groups. For example, alkyl ether sulfate anionic surfactants can contain less than 5 moles, or less than 4 moles, of ethylene oxide groups, for example, 1 to 4 or 2 to 3 ethylene oxide groups. A single anionic surfactant can be used, or multiple anionic surfactants (for example, 2, 3, 4 or more) can be used.

[0028] In various embodiments, suitable nonionic surfactants can include alkyl ethoxylate condensation products of aliphatic alcohols with 1 to 25 moles of ethylene oxide, where the alkyl chain of the aliphatic alcohol can be straight or branched, primary or secondary, and generally contains 6 to 22 carbon atoms. Further suitable nonionic surfactants include water-soluble ethoxylated C6-C 18 Aliphatic alcohols and C6-C 18 Mixed ethoxylated / propoxylated fatty alcohols. For example, the ethoxylated fatty alcohols are C 3 fatty alcohols with a degree of ethoxylation of 3 to 20. 10 -C 18The nonionic surfactant may be an ethoxylated fatty alcohol. In some embodiments, the mixed ethoxylated / propoxylated fatty alcohol may have an alkyl chain length of 10 to 18 carbon atoms, an ethoxylation degree of 3 to 30, and a propoxylation degree of 1 to 10. In further embodiments, suitable nonionic surfactants may include those formed from the condensation of ethylene oxide with a hydrophobic base formed by the condensation of propylene oxide and propylene glycol. Compounds of this type include, for example, certain commercially available Pluronic™ surfactants (sold by BASF). Furthermore, suitable nonionic surfactants may include those formed from the condensation of ethylene oxide with the product obtained by the reaction of propylene oxide and ethylenediamine. Nonionic surfactants of this type include, for example, certain commercially available Tetronic™ compounds (sold by BASF). In some embodiments, suitable nonionic surfactants may be selected from, for example, various alcohol ethoxylates. In some embodiments, nonionic surfactants may be defined in terms of the alcohol chain length and / or the number of ethoxylate groups present in the molecule. For example, the nonionic surfactant may include an alcohol ethoxylate formed from an alcohol having a carbon chain length of 3 to 20 carbon atoms, 5 to 20 carbon atoms, 7 to 19 carbon atoms, 9 to 18 carbon atoms, 10 to 17 carbon atoms, or 12 to 15 carbon atoms. By way of further example, the nonionic surfactant may include an alcohol ethoxylate having 2 to 10, 4 to 9, or 6 to 8 moles of ethylene oxide per mole of alcohol. Non-limiting examples of nonionic surfactants that may be used in the present invention include ethoxylated alcohols (AE), particularly C 12-15 alcohols), such as those available under the trade name NEODOL® (particularly available as NEODOL® 25-7), lauryl or myristyl glucoside (APG), and polyoxyethylene alkyl ether (2° AE). A single nonionic surfactant can be used, or multiple nonionic surfactants (e.g., 2, 3, 4 or more) can be used.

[0029] Suitable builders useful as detergent ingredients can be effective as alkalizing agents. For example, various alkali carbonates and / or other inorganic alkalizing agents can be used. Preferably, sodium and / or potassium salts (e.g., K2CO3 and / or Na2CO3) can be used. For example, soda ash can be used. In some embodiments, one or more ingredients can be used for in-situ carbonate formation. For example, a combination of bicarbonate and hydroxide can be effective for in-situ carbonate formation. In one example embodiment, sodium bicarbonate and sodium hydroxide can be used for this purpose, although other forms of bicarbonate and hydroxide can be used as well.

[0030] The cleaning agent component can be a peroxide precursor composition. For example, sodium percarbonate, which is an adduct of hydrogen peroxide complexed with sodium carbonate, can be used. Such materials can be characterized as "bleaching agents" in relation to their stain removal ability, or as brighteners or brighteners.

[0031] In one or more embodiments of the present disclosure, the unit dose composition may include a plasticizer. The plasticizer may be any material that is effective in improving the bond between the structuring agent and the alcoholate complex component. For example, the plasticizer may be a material that at least partially solvates a polymer useful as a structuring agent, increasing the bond between the polymer and the salt / alcohol matrix. Thus, the plasticizer may be characterized as an organic solvent. The solubility of the structuring agent in the plasticizer can be estimated using the solubility parameter theory already described above. In some embodiments, the difference in δ between the solvent (plasticizer) and the solute (structuring agent) is less than 7 (MPa). 1 / 2 The plasticizer can therefore be less than about 1 (MPa) 1 / 2 to approximately 6.9 (MPa) 1 / 2 , approximately 1.5 (MPa) 1 / 2 to approximately 6.8 (MPa) 1 / 2 , or about 2 (MPa) 1 / 2 to approximately 6.5 (MPa) 1 / 2In a further embodiment, the difference in solubility parameters may be in the range of 7 (MPa) 1 / 2 Less than 6.8 (MPa) 1 / 2 Less than 6.5 (MPa) 1 / 2 Less than 6 (MPa) 1 / 2 Less than or 5.5 (MPa) 1 / 2 In further embodiments, the plasticizer can be any material having a relatively low volatility, which can be determined based on vapor pressure, which can be measured using known experimental methods or calculated using known equations. For example, the plasticizer can have a vapor pressure of less than 12 mm Hg (about 1600 Pa), less than 10 mm Hg (about 1333 Pa), less than 8 mm Hg (about 1067 Pa), less than 5 mm Hg (about 667 Pa), or less than 3 mm Hg (about 400 Pa), measured at 20° C.

[0032] In some embodiments, the vapor pressure can be from about 0.0001 mm Hg (about 0.0133 Pa) to about 10 mm Hg (about 1333 Pa), from about 0.0001 mm Hg (about 0.0133 Pa) to about 6 mm Hg (800 Pa), or from about 0.0001 mm Hg (about 0.0133 Pa) to about 4 mm Hg (about 533 Pa), measured at 20°C.

[0033] In an exemplary embodiment, the plasticizer can be a glycol ether, such as diethylene glycol hexyl ether (also known as hexyl carbitol). For example, diethylene glycol hexyl ether exhibits a vapor pressure of 0.001 mm Hg at 20° C., compared to 6.6 (MPa) for S630 Plasdone polymer, which is just one example of a polymer useful as a structuring agent according to the present disclosure. 1 / 2This results in a difference value of δ between the hardness and deformability of the unit dose composition. The activity of the plasticizer can be effective to increase deformation of the unit dose solid by softening the structurant. However, excessive plasticizer can undesirably reduce hardness. It is beneficial to create a balance between hardness and deformability in the unit dose composition to provide toughness, so that the unit dose composition resists breakthrough deformation, but resists excessive deformation in view of hardness.

[0034] In some embodiments, unit dose compositions according to the present disclosure may comprise about 0.1% to about 5%, about 0.5% to about 4.5%, or about 1% to about 4% by weight of plasticizer, based on the total weight of the unit dose composition. In further embodiments, the unit dose composition may comprise at least 0.1%, at least 0.2%, at least 0.5%, or at least 1.0% by weight of plasticizer, based on the total weight of the unit dose composition. In such embodiments, an upper limit (i.e., less than or equal to) may apply, for example, an upper limit of 10%, 8%, or 5% by weight, based on the total weight of the unit dose composition.

[0035] In the present disclosure, the unit dose composition is configured as a monolithic solid. In this embodiment, the monolithic solid is distinguished from powders or other solid formats that exist as multiple smaller particles that do not remain bound together as a larger unit dose format. However, in some embodiments, the unit dose composition can be characterized as a pellet, disc, puck, tablet, or the like, which is understood to be a single monolithic solid object of sufficient size to provide a useful amount of the cleaning agent ingredients. For example, the unit dose composition of the present disclosure can have a length, width, and thickness, each independently within the range of about 1 cm to about 10 cm, about 1.5 cm to about 8 cm, or about 2 cm to about 6 cm. Similarly, for a substantially spherical or ellipsoidal shape, the single unit dose composition can have an average diameter of about 2 cm to about 10 cm, about 2.5 cm to about 8 cm, or about 3 cm to about 6 cm.

[0036] The unit dose composition's monolithic solid form may exhibit a structure that will not separate unless significant force exceeding its tolerance is applied to the solid structure. The monolithic solid may be a rigid structure, but also possess a sufficient degree of deformation to resist fracture under the applied force. In some embodiments, the monolithic solid has a hardness value defined by exhibiting a peak force at break of at least 100 Newtons, at least 120 Newtons, at least 150 Newtons, at least 170 Newtons, or at least 190 Newtons. The monolithic solid may also have a percent deformation at peak force of about 5% to about 50%, about 10% to about 40%, or about 20% to about 30%. Hardness and deformation can be assessed by any acceptable method. For example, such values ​​can be obtained by standard operation of a texture analyzer, such as those available from Brookfield Ametek. In one exemplary embodiment, a blade attached to the texture analyzer can be lowered toward a test material (e.g., a monolithic solid composition according to the present disclosure) at a specified speed, e.g., about 0.50 mm / s. The peak force can be identified as the point at which failure of the monolithic solid occurs, and the percent deformation can be identified based on how far the blade penetrates into the monolithic solid before failure occurs.

[0037] As already mentioned above, conventional unit dose compositions require a film or envelope to encase the materials and maintain them in a unit dose form. In the present disclosure, the unit dose composition is configured as a monolithic solid, which does not require a film or envelope to conform to the structure of the composition. Even in the absence of such additional enveloping materials, the unit dose composition in the form of a monolithic solid effectively retains its originally formed shape and mass until use by the consumer. Upon use, the unit dose composition is preferably water-soluble. In some embodiments, the monolithic solid is configured to achieve at least 95% dissolution in deionized water in a time period of about 30 seconds to about 8 minutes, about 1 minute to about 7 minutes, or about 2 minutes to about 6 minutes. Dissolution is evaluated as the time to achieve about 95% solubilization of the unit dose by weight in deionized water. Dissolution can be tested, for example, by placing the monolithic solid in 1 liter of deionized water at a temperature of about 22°C and stirring at 300 revolutions per minute (rpm) until the article begins to solubilize in the water, as assessed by visual inspection. As described herein, the dissolution time may vary depending on the water temperature. Dissolution is important for releasing the active ingredients in the integrated solid, for example, to release laundry detergent materials in a washing machine so that cleaning can occur. A shorter dissolution time leads to better cleaning performance, as the active ingredients are exposed to laundry for a longer period of time, effectively cleaning the laundry. Preferably, the composition exhibits a dissolution time of less than 12 minutes, less than 10 minutes, less than 8 minutes, or less than 6 minutes when tested under the above conditions. For example, the exhibited dissolution time may be about 0.5 minutes to about 10 minutes, about 1 minute to about 9 minutes, or about 2 minutes to about 8 minutes. As further described in Example 1 and Example 8, the integrated solid dissolution time can be measured by equating the dissolution time of a commercially available laundry unit dose in a polyvinyl alcohol pouch with liquid.

[0038] The unit dose composition preferably contains little or no water. Because matrix formation relies on the reaction between the alcohol and the anhydrous salt, it is beneficial to limit the water content to limit competition for reaction with the anhydrous salt. In some embodiments, the unit dose composition may contain less than 5 wt.%, less than 4 wt.%, less than 3 wt.%, less than 2 wt.%, less than 1 wt.%, or less than 0.5 wt.% water, based on the total weight of the final unit dose composition. Preferably, water is not intentionally added to the unit dose composition, although small amounts of water may be present due to the inclusion of other ingredients (e.g., surfactants) or certain decomposition reactions that generate water, such as the decomposition of sodium percarbonate. The unit dose composition may thus be described excluding added water, which may be defined as free water added to the composition as an independent material, as opposed to a chemical component of other materials used in the composition.

[0039] In one or more embodiments, the present disclosure may further provide a method for making a unit-dose composition. The method may generally include preparing a premix of less than all of the components of the composition and then adding at least one additional component of the composition effective to initiate a reaction to form a complex. For example, a method according to the present disclosure may include combining a structuring agent, a detergent, and an alcohol to form a mixture. The method may further include combining the mixture with an anhydrous salt to form an intermediate composition. The method may also include curing the unit-dose amount of the intermediate composition under conditions where the anhydrous salt reacts with the alcohol to form a complex. The complex structurally includes the structuring agent and the detergent to provide the unit-dose amount as a discrete unit of a cohesive solid. In some embodiments, the combining further includes combining a plasticizer to form the mixture. [Example]

[0040] Example 1 The test compositions were prepared by first preparing a Part A mixture containing alcohol, polymer, plasticizer, and surfactant effective as a laundry detergent. The formula for the Part A mixture is shown in Table 1 below.

[0041] [Table 1]

[0042] A 60.98 weight percent (wt%) amount of the Part A mixture was then combined with 39.02 wt% of the anhydrous salt calcium chloride. The combined materials formed a soft, dough-like intermediate material, which was pressed into a silicone mold. The silicone mold formed a unit-dose "block" measuring 40 mm x 40 mm x 20 mm with a mass weight of approximately 20 grams (g). Within 5 minutes of the intermediate mixture solidifying in the mold, a monolithic solid was formed. The overall formulation is shown below in Table 2.

[0043] [Table 2]

[0044] After formation of the unit dose composition, the integrated solid was tested for dissolution. To be effective, the unit dose composition should exhibit solubility characteristics comparable to conventional unit dose compositions contained in envelopes, films, or other forms. One liter of deionized water at a temperature of 22 degrees Celsius (°C) was placed in a 1500 milliliter (ml) beaker and stirred at 300 revolutions per minute (rpm) using a magnetic stir bar (3 / 8" x 2.5") . Complete dissolution was observed approximately 6 minutes after the integrated solid was placed in the water. As described herein, dissolution time may vary depending on water temperature. A typical wash cycle is on the order of about 10 to about 12 minutes in length. Thus, the target dissolution time for the integrated solid is less than 12 minutes, leaving sufficient time for the active ingredients to be exposed to the fabric so that cleaning can occur. Preferably, the dissolution time is less than about 8 minutes, as shorter times result in better cleaning performance. To compare the dissolution of the unit dose compositions described herein with that of a commercially available laundry unit dose in a polyvinyl alcohol pouch, the dissolution of the commercial laundry unit dose was measured at about 6.5 minutes into the wash cycle, at which point the polymer had completely dissolved into the wash water.However, the pouch rupture, accompanied by the release of the active ingredient, occurred at about 2.5 minutes.

[0045] Example 2 Eight separate unit dose compositions were prepared to test the formation of matrices formed between different anhydrous salts and alcohols. For testing, 2-propanol was used as the alcohol. The anhydrous salts tested included magnesium chloride (MgCl), calcium chloride (CaCl), strontium chloride (SrCl), and barium chloride (BaCl). The unit dose compositions prepared using the Part A mixture from Example 1 and anhydrous salts are shown in Table 3 below (values ​​are in weight percent).

[0046] [Table 3]

[0047] The components of each of the unit dose compositions, including alcohol, structurant, plasticizer, detergent, and anhydrous salt, are shown in Table 4 below (values ​​are in weight percent).

[0048] [Table 4]

[0049] Compositions 97-1c, 97-1d, 97-2c, and 97-2d did not produce a rigid structure, but instead formed a soft paste or dispersion that separated. Of the test samples, those formed using MgCl and CaCl formed the desired monolithic solid unit dose compositions. Without wishing to be bound by theory, this result is believed to result from the different electronegativities of the cation components of the anhydrous salts tested.

[0050] Next, a dissolution test was performed. One liter of deionized water at a temperature of 22°C was placed in a 1500 ml beaker and stirred at 300 rpm using a magnetic stir bar (3 / 8" x 2 1 / 2"). The complete dissolution time (minutes) after the test composition that formed the integrated solid structure was placed in water is shown in Table 5 below.

[0051] [Table 5]

[0052] Example 3 Part A3 mixtures were prepared with alcohol, structurant, plasticizer and surfactant (values ​​in wt%). Example formulations are shown in Table 6 below.

[0053] [Table 6]

[0054] Part A3 was then mixed with MgCl or CaCl to form a unit dose composition with a monolithic solid structure. Samples 98-lc and 98-ld also contained a detergent (sodium dodecyl sulfate) as shown in Table 7 below (values ​​are in wt%).

[0055] [Table 7]

[0056] The overall weight percentages of the components of the unit dose compositions for Samples 98-1a, 98-1b, 98-1c and 98-1d are shown in Table 8 below.

[0057] [Table 8]

[0058] Dissolution testing was completed after sample formation. One liter of deionized water at a temperature of 22°C was placed in a 1500 ml beaker and stirred at 300 rpm using a magnetic stir bar (3 / 8" x 2 1 / 2"). The complete dissolution times (in minutes) for samples 98-1a, 98-1b, 98-1c, and 98-1d after placing them in water are shown in Table 9 below.

[0059] [Table 9]

[0060] Example 4 Tests were conducted to evaluate the effect that varying the ratio of structurant and anhydrous salt components had on the physical properties of the unit dose compositions formed. Seven test samples were evaluated, as shown in Table 10 below (values ​​are wt %).

[0061] [Table 10]

[0062] Solid unit packs were prepared as described in Example 1. Packs were cut to an approximate size of 4 cm (length) x 4 cm (length) x 2 cm (height). The hardness value of each pack was evaluated using a Brookfield texture analyzer. The unit dose pack was placed on a platform beneath a tapered plastic blade (Brookfield geometry TA7) measuring 6 cm (width) x 5 cm (height) x 0.3 cm (width). The blade was lowered toward the pack at 0.50 mm / s while recording force as a function of time and position. The parameters recorded were peak force and percent deformation, defined as the percent penetration depth relative to the pack height at the peak force. The peak force was identified as the point at which pack failure occurred. The percent deformation was determined based on how far the blade penetrated into the pack before failure occurred.

[0063] The peak force and percent deformation values ​​are shown below in Table 11. In Figure 2, the peak force (hardness) values ​​are plotted against the ratio of structurant concentration to anhydrous salt concentration. In Figure 3, the percent deformation values ​​are plotted against the ratio of structurant concentration to anhydrous salt concentration.

[0064] [Table 11]

[0065] The test results show that composition 5632-4-2, which did not contain a polymer, lacked structural integrity and was unable to form a well-defined shape. The force for composition 5632-4-2 was therefore recorded as 0. Composition 5632-4-3 had a shape but exhibited relatively low peak force and deformation before fracture. The results for both composition 4-2 and composition 4-3 are shown in Figures 2 and 3.

[0066] As shown in Table 11, the inclusion of a structurant was effective not only in binding the components into a defined shape, but also in providing structural integrity to the composition. A peak in hardness value was observed at a structurant to anhydrous salt ratio of around 0.29. A peak in % deformation was observed at a slightly lower ratio of 0.12, but this value was similar to the value at the 0.29 ratio. This indicated that the ratio of the two components could be adjusted to optimize hardness and deformation. Optimal hardness and deformability are properties related to product integrity; for example, products may be subjected to rough handling during shipping.

[0067] Example 5 Tests were conducted to identify the effect of varying the amount of plasticizer present in the unit dose composition. Compositions containing different levels of hexyl carbitol (C6E2, diethylene glycol hexyl ether) were prepared, as shown in Table 12 below (values ​​are in wt %).

[0068] [Table 12]

[0069] The compositions were tested on a Texture Analyzer as described above. Peak force (hardness) and percent deformation data are shown in Figures 4 and 5, respectively. The data is also shown in Table 13. Figure 4 is a graph depicting peak force (hardness) values ​​plotted against weight percent plasticizer. FIG. 5 is a graph depicting percent deformation at peak force (hardness) values ​​plotted against weight percent of plasticizer.

[0070] [Table 13]

[0071] Tests have shown that plasticizers can be beneficial for improving hardness, possibly by sufficiently plasticizing the structurant polymer so that it can interact and bond with other components of the solid matrix. However, excessive plasticizer content can further increase deformation but reduce peak hardness force. Thus, plasticizer content can be beneficial for customizing deformation characteristics as needed.

[0072] Example 6 Additional tests were conducted to evaluate the cleaning efficacy of the unit dose compositions. Table 14 describes compositions prepared with varying levels of sodium percarbonate (NaPC) included as a cleaning ingredient.

[0073] [Table 14]

[0074] The compositions in Table 14 were evaluated for wash performance by adding two packs (approximate size: 4 cm x 4 cm x 2 cm) to a total wash (approximately 70 L) containing test flags with the stains and soils shown in Table 15. In Table 15, "C" refers to stains on cotton flags and "PC" refers to stains on cotton-blend polyester flags.

[0075] [Table 15]

[0076] Cleaning was performed at 86°F using wash water with a hardness of 120 ppm (parts per million) (as CaCO3). Cleaning efficacy was assessed by comparing color assessments of the stains before and after cleaning. The color was evaluated by the CIE L*a*b* color space (HunterLab, Application Note Vol. 8, No. 7, July 1996) and the color was evaluated by image analysis for the unwashed and washed stains. The root mean square ΔE value of the color difference between the cloth and an unstained reference cloth was then calculated for the unwashed cloth according to Equation 1 shown below and for the washed cloth according to Equation 2 shown below: Before washing: ΔE U =[(L u -L o ) 2 +(a u -a o ) 2 +(b u -b o ) 2 ] 1 / 2 ...Formula 1 After washing: ΔE W =[(L w -L o ) 2 +(a w -a o ) 2 +(b w -b o ) 2 ] 1 / 2 ...Formula 2 where u, w, and o correspond to the values ​​for the unwashed, washed, and unstained cloths, respectively. The percent stain removal (%SR) was then calculated according to Equation 3 shown below. %SR=[(ΔE U -ΔE W ) / ΔE U ]×100...expression 3 A composite cleaning performance score was calculated by summing the %SR scores for each stain. The composite scores from the commercial laundry detergent, the commercial laundry sheet product, and the three experimental products are compared in Table 16 below.

[0077] [Table 16]

[0078] The cleaning results showed that the inventive sample performed well compared to the current cleaning system. Increasing the level of sodium percarbonate improved cleaning performance.

[0079] Example 7 To measure dissolution times between compositions, the following two compositions were prepared. In these formulations, the alcohol to salt ratio was varied. The other ingredients remained constant.

[0080] [Table 17]

[0081] The dissolution time for composition 15-1, which had a higher alcohol / salt ratio, was measured to be 1.25 minutes, while the dissolution time for composition 16-1, which had a lower alcohol / salt ratio, was measured to be 2.5 minutes. As shown, increasing the alcohol to salt ratio was found to decrease the dissolution time of the solid unit dose composition.

[0082] Example 8 The elution times for two compositions made with vinyl acetate / vinylpyrrolidone (Vac / VP) copolymers of different chemical compositions were compared. The Plasdone S630 copolymer had a molecular weight of 43,000 g / mol and a VAc / VP ratio of 1.5. An additional VAc / VP polymer obtained from Aldrich Chemical had a MW of 50,000 g / mol and a VAc / VP ratio of 1.3. The two compositions are shown in Table 18 below.

[0083] [Table 18]

[0084] The dissolution time for composition 15-1 with Plasdone 630 polymer was measured to be 1.25 minutes, while the dissolution time for composition 12-2 with Aldrich Vac / VP polymer was measured to be 2.5 minutes.

[0085] As used herein, the terms "about" or "substantially" are intended to indicate that the value or condition referred to encompasses both the explicitly stated value or condition and values ​​relatively close thereto or conditions that are perceived to be relatively close thereto. For example, unless otherwise indicated herein, a numerical value preceded by "about" or a "substantially" value can refer to a particular number or value and a number or value that varies therefrom (+ or -) by 5% or less, 4% or less, 3% or less, 2% or less, or 1% or less, and any one of such values ​​can be used interchangeably with the words "about" and / or "substantially," used as needed for clarity. Similarly, unless otherwise indicated herein, a condition that is substantially present can indicate that the condition is met exactly as stated or claimed, is within typical manufacturing tolerances, or that the required condition appears to be met upon casual observation even if the required condition is not completely met. In some embodiments, a value or condition can be defined as expressed, and thus the terms "about" or "substantially" (and the variations as described) can be excluded from the expressed value.

[0086] Numerous modifications and other embodiments of the disclosures set forth herein will come to mind for those skilled in the art using the teachings set forth in the foregoing description. It is therefore understood that the disclosure is not limited to the particular embodiments disclosed, and that modifications and other embodiments are intended to be included within the scope of the appended claims. Although specific terms are used herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims

1. a complex of an alcohol and an anhydrous salt; a structuring agent; and Cleaning agent and 1. A unit dose composition comprising:

2. 10. The unit dose composition of claim 1, wherein the alcohol is present in an amount of about 30% to about 45% based on the total weight of the unit dose composition.

3. 2. The unit dose composition of claim 1, wherein the anhydrous salt is an anhydrous chloride salt.

4. 4. The unit dose composition of claim 3, wherein the anhydrous salt comprises a cation having an electronegativity of at least 1.

0.

5. 10. The unit dose composition of claim 1, wherein the anhydrous salt is present in an amount of about 30% to about 45% by weight based on the total weight of the unit dose composition.

6. The unit dose composition of claim 1 , wherein the structuring agent comprises a polymer.

7. 7. The unit dose composition of claim 6, wherein the structuring agent comprises an acetate polymer.

8. 7. The unit dose composition of claim 6, wherein the structuring agent comprises a copolymer of acetate monomer and one or more additional monomers.

9. 10. The unit dose composition of claim 1, wherein the structuring agent is present in an amount of about 5% to about 20% by weight based on the total weight of the unit dose composition.

10. 10. The unit dose composition of claim 1, further comprising a plasticizer.

11. 11. The unit dose composition of claim 10, wherein the plasticizer is a liquid that is effective to partially solubilize the structuring agent and increase the bonding of the structuring agent with the alcohol and anhydrous salt complex.

12. 11. The unit dose composition of claim 10, wherein the plasticizer comprises glycol hexyl ether.

13. 11. The unit dose composition of claim 10, wherein the plasticizer is present in an amount of about 0.1% to about 5% by weight based on the total weight of the unit dose composition.

14. 14. The unit dose composition of claim 1, wherein the cleaning agent is selected from the group consisting of surfactants, builders, alkalizing agents, enzymes, optical brighteners, anti-redeposition polymers, optical brighteners, bleaching agents, pearlescent agents, and combinations thereof.

15. 14. The unit dose composition of any of claims 1 to 13, wherein the monolithic solid has a hardness value defined by exhibiting a peak force at break of at least 190 Newtons and a percent deformation at peak force of about 20% to about 30%, as measured with a texture analyzer.

16. 14. A unit dose composition according to any preceding claim, wherein the monolithic solid is not partially or completely enclosed in a film or envelope.

17. 14. The unit dose composition of claim 1, wherein the monolithic solid is water-soluble.

18. 18. The unit dose composition of claim 17, wherein the monolithic solid is configured to achieve at least 95% dissolution in deionized water in a time period of about 30 seconds to about 8 minutes.

19. combining a structurant, a detergent, and an alcohol to form a mixture; combining said mixture with an anhydrous salt to form an intermediate composition; curing the unit dose amount of said intermediate composition under conditions such that said anhydrous salt reacts with said alcohol to form a complex structurally comprising said structuring agent and said cleaning agent to obtain the unit dose amount as a discrete unit of a cohesive solid; A method of making a unit dose composition comprising:

20. 20. The method of claim 19, wherein said combining further comprises combining a plasticizer to form said mixture.

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