Methods of Making and Using Aqueous Cotton Reclaiming Compositions

Abstract

1. A method of making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics, comprising providing a liquid carrier; providing a cellulase; and selecting a protectant polymer, the protectant polymer comprising 25 to 65 weight percent, based on the weight of the protectant polymer, of structural units of formula (I), where each R is independently selected from hydrogen and a —CH group, and 35 to 75 weight percent, based on the weight of the protectant polymer, of structural units of formula (II), where each R 2 -C 2~3 alkyl groups, and each R 3 is independently selected from hydrogen and methyl groups), providing the selected protectant polymer, and combining a liquid carrier, cellulase, and the selected protectant polymer to form an aqueous cotton regenerating composition. A method for regenerating soiled cotton-containing fabrics is also provided. [Formula 1] JPEG2023529086000016.jpg28128

Description

[Technical Field]

[0001] The present disclosure relates to a method for making an aqueous cotton regeneration composition. In particular, the present invention relates to a method for making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics, the method comprising providing a liquid carrier, providing a cellulase, and selecting a protectant polymer, the protectant polymer comprising 25 to 65 weight percent of structural units of formula I, based on the weight of the protectant polymer.

[0002] [ka] (In the formula, each R 1 are independently selected from hydrogen and —CH groups), and 35 to 75 wt. % of structural units of formula II, based on the weight of the protectant polymer.

[0003] [ka] (In the formula, each R 2 -C 2~3 alkyl groups, and each R 3 wherein R is independently selected from hydrogen and methyl groups, providing the selected protectant polymer, and combining a liquid carrier, cellulase, and the selected protectant polymer to form an aqueous cotton regenerating composition. The present invention also relates to a method for regenerating soiled cotton-containing fabrics. [Background technology]

[0004] Enzymes (e.g., cellulases) are increasingly considered desirable for inclusion in cleaning formulations. However, these cleaning formulations have historically suffered from problems, such as chemical instability, which results in the loss of enzyme activity. This loss of enzyme activity is more pronounced in liquid and gel compositions. Enzymes can be destabilized in these formulations by unfolding the enzyme's three-dimensional structure or by degrading the enzyme. Common destabilizing factors include polar solvents such as water or other solvents, microbial attack, electrolytes, charged surfactants, temperature, and pH extremes. This instability becomes even more problematic during storage. The loss of enzyme activity during storage has led to more limited adoption of certain enzymes in the liquid detergent industry. It is not uncommon for certain products to be stored in warehouses in various climates around the world, and a given product may be subjected to temperatures that can range from freezing to over 40°C for extended periods of time. When stored under such temperature extremes for periods of several weeks, many liquid enzyme compositions lose 20 to 100 percent of their enzyme activity due to enzyme instability.

[0005] To compensate for the loss of enzyme activity during storage, formulators may resort to using excess enzyme in the formulation. Enzymes are relatively expensive formulation ingredients. Therefore, formulators have sought to use enzyme stabilizers in liquid compositions to inhibit enzyme destabilization reactions.

[0006] One approach to stabilizing enzyme-containing formulations is described by Lenoir in U.S. Patent No. 8,110,539. Lenoir discloses a method for stabilizing a liquid enzyme-containing liquid formulation by adding at least one boron compound and at least one alpha-hydroxy-monocarboxylic acid or salt of an alpha-hydroxy-monocarboxylic acid capable of forming an enzyme-stabilizing compound.

[0007] Nevertheless, there remains a need for aqueous cotton regenerating compositions that exhibit enzymatic stability upon storage at elevated temperatures for extended periods of time, and methods of making and using the same. Summary of the Invention

[0008] The present invention provides a method for making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics, comprising providing a liquid carrier; providing a cellulase; and selecting a protectant polymer, wherein the protectant polymer comprises 25 to 65 weight percent of structural units of formula I, based on the weight of the protectant polymer.

[0009] [ka] (In the formula, each R 1 are independently selected from hydrogen and —CH groups), and 35 to 75 wt. % of structural units of formula II, based on the weight of the protectant polymer.

[0010] [ka] (In the formula, each R 2 -C 2~3 alkyl groups, and each R 3 is independently selected from hydrogen and a methyl group), providing the selected protectant polymer, and combining a liquid carrier, cellulase, and the selected protectant polymer to form an aqueous cotton regenerating composition.

[0011] The present invention provides a method for making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics, comprising providing a liquid carrier; providing a cellulase; and selecting a protectant polymer, wherein the protectant polymer contains 25 to 65 weight percent, based on the weight of the protectant polymer, of structural units of formula I, where each R 1 are independently selected from hydrogen and —CH groups), and 35 to 75 weight percent structural units of formula II, based on the weight of the protectant polymer, 2 -C 2~3 alkyl groups, and each R 3is independently selected from hydrogen and a methyl group), providing the selected protectant polymer, combining a liquid carrier, a cellulase, and the selected protectant polymer to form an aqueous cotton regeneration composition, providing a soiled cotton-containing fabric, providing wash water, providing rinse water, contacting the soiled cotton-containing fabric with the aqueous cotton regeneration composition and the wash water to provide a regenerated cotton-containing fabric, and contacting the regenerated cotton-containing fabric with rinse water to rinse away the regeneration composition. DETAILED DESCRIPTION OF THE INVENTION

[0012] Surprisingly, it has been found that aqueous liquid laundry formulations of the present invention containing protectant polymers and cellulases exhibit improved anti-redeposition performance on cotton-containing fabrics after extended storage (i.e., 7 weeks) at ≥ 40°C (preferably 40°C).

[0013] Unless otherwise indicated, ratios, percentages, parts, etc. are by weight. Weight percentages (or wt %) in a composition are percentages of dry weight, i.e., excluding any water that may be present in the composition.

[0014] As used herein, unless otherwise indicated, "weight average molecular weight" and "M w The term "weight average molecular weight" is used interchangeably to refer to weight average molecular weight measured in the conventional manner using gel permeation chromatography (GPC) and conventional standards such as polystyrene standards. GPC techniques are discussed in detail in *Modern Size Exclusion Liquid Chromatography: Practice of Gel Permeation and Gel Filtration Chromatography*, Second Edition, Striegel, et al., John Wiley & Sons, 2009. Weight average molecular weights are reported herein in units of Daltons.

[0015] The term "structural unit" as used in this specification and the appended claims refers to the remnant of the indicated monomer, thus indicating a structural unit of (meth)acrylic acid:

[0016] [ka] where the dotted lines represent points of attachment to the polymer backbone and R 1 is the hydrogen in the structural unit of acrylic acid and the -CH3 group in the structural unit of methacrylic acid.

[0017] Preferably, the method of making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics of the present invention comprises providing a liquid carrier; providing a cellulase; and selecting a protectant polymer, the protectant polymer comprising 25 to 65 wt. % (preferably, 30 to 60 wt. %, more preferably, 35 to 55 wt. %, and most preferably, 40 to 44 wt. % of structural units of Formula I, based on the weight of the protectant polymer.

[0018] [ka] (In the formula, each R 1 are independently selected from hydrogen and —CH groups), and 35 to 75 wt % (preferably 40 to 70 wt %, more preferably 45 to 65 wt %, and most preferably 56 to 60 wt %) of structural units of formula II, based on the weight of the protectant polymer.

[0019] [ka] (In the formula, each R 2 -C 2~3 alkyl groups, and each R 3are independently selected from hydrogen and methyl groups) (preferably, the protectant polymer is selected based on its cellulase protection ability, more preferably, the protectant polymer is selected based on its cellulase protection ability as demonstrated by the anti-redeposition performance of the aqueous cotton regeneration composition after storage in a closed container at ≥ 40°C (preferably 40-90°C) for 7 weeks), providing the selected protectant polymer; and combining the liquid carrier, cellulase, and the selected protectant polymer to form the aqueous cotton regeneration composition.

[0020] Preferably, the method of making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics of the present invention optionally further comprises providing an additional ingredient selected from the group consisting of at least one of a detersive surfactant (e.g., linear alkylbenzene sulfonic acid), an organic solvent (e.g., ethanol, propylene glycol, monoethanolamine (MEA)), a structurant, a hydrotrope (e.g., sodium xylene sulfonate), a fragrance, a foam control agent (e.g., fatty acid, polydimethylsiloxane), a builder (trisodium citrate dihydrate), and a fabric softener; and combining the additional ingredient with a liquid carrier, cellulase, and a selected protectant polymer to form the aqueous cotton regeneration composition.

[0021] Preferably, the method for making the aqueous cotton regeneration composition for regenerating soiled cotton-containing fabric of the present invention is a method for regenerating soiled cotton-containing fabric, and further comprises providing a soiled cotton-containing fabric, providing wash water, providing rinse water, contacting the soiled cotton-containing fabric with the aqueous cotton regeneration composition and the wash water to provide a regenerated cotton-containing fabric, and contacting the regenerated cotton-containing fabric with rinse water to rinse away the regeneration composition (preferably, sufficient protective polymer is provided so that the cellulase concentration in the wash water is 0.005 to 1.0 ppm by mass (more preferably, 0.02 to 0.5 ppm by mass)). More preferably, the method of making the aqueous cotton regeneration composition for regenerating a soiled cotton-containing fabric of the present invention is a method of regenerating a soiled cotton-containing fabric, further comprising: aging the aqueous cotton regeneration composition at ≥40°C (preferably 40-90°C) for at least 7 weeks (preferably 7-12 weeks, more preferably 7-10 weeks, most preferably 7-8 weeks) to form an aged aqueous cotton regeneration composition; providing a soiled cotton-containing fabric; providing wash water; providing rinse water; contacting the soiled cotton-containing fabric with the aged aqueous cotton regeneration composition and the wash water to provide a regenerated cotton-containing fabric; and contacting the regenerated cotton-containing fabric with rinse water to rinse off the aged aqueous regeneration composition (preferably providing sufficient protective polymer such that the cellulase concentration in the wash water is 0.005-1.0 ppm by mass (more preferably 0.02-0.5 ppm by mass)).

[0022] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises a liquid carrier (preferably 25 to 99.949 wt % (more preferably 30 to 99.89 wt %, even more preferably 35 to 99.7 wt %, most preferably 40 to 60 wt %) of the liquid carrier, based on the weight of the aqueous cotton regeneration composition), and a cellulase (preferably 0.001 to 2 wt % (more preferably 0.01 to 1 wt %, even more preferably 0.05 to 0.5 wt %, most preferably 0.07 to 10 wt %) of a cellulose acetate solution ... and a protectant polymer (preferably 0.05 to 5 wt. % (more preferably 0.1 to 3 wt. %, even more preferably 0.25 to 2.0 wt. %, and most preferably 0.4 to 1 wt. % of the protectant polymer, based on the weight of the aqueous cotton regenerating composition), wherein the protectant polymer comprises 25 to 65 wt. % (preferably 30 to 60 wt. %, more preferably 35 to 55 wt. %, and most preferably 40 to 44 wt. % of a structural unit of formula I (wherein each R 1 are independently selected from hydrogen and —CH groups), and 35 to 75 wt % (preferably 40 to 70 wt %, more preferably 45 to 65 wt %, and most preferably 56 to 60 wt %) of structural units of formula II, based on the weight of the protectant polymer, 2 -C 2~3 alkyl groups (preferably -C alkyl groups), and each R 3 are independently selected from hydrogen and methyl groups (preferably hydrogen).

[0023] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises a liquid carrier. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises 25 to 99.949 wt % (preferably, 30 to 99.89 wt %, more preferably, 35 to 99.7 wt %, and most preferably, 40 to 60 wt %) of the liquid carrier, based on the weight of the aqueous cotton regeneration composition. Even more preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises 25 to 99.949 wt % (preferably, 30 to 99.89 wt %, more preferably, 35 to 99.7 wt %, and most preferably, 40 to 60 wt %) of the liquid carrier, based on the weight of the aqueous cotton regeneration composition, and the liquid carrier comprises water. Most preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises 25 to 99.949 wt % (preferably, 30 to 99.89 wt %, more preferably, 35 to 99.7 wt %, and most preferably, 40 to 60 wt %) of the liquid carrier, based on the weight of the aqueous cotton regeneration composition, and the liquid carrier is water.

[0024] Preferably, the liquid carrier is, optionally, C 1~3 Alkanolamines (e.g., monoethanolamine), C 1~3 Alkanols (e.g., ethanol), and C 1~3 More preferably, the liquid carrier optionally comprises 0 to 20 wt. % (preferably 1 to 17.5 wt. %, more preferably 2.5 to 15 wt. %, and most preferably 5 to 12 wt. %) of a water-miscible liquid, based on the weight of the liquid carrier, and the water-miscible liquid is selected from the group consisting of C 1~3 Alkanolamines, C 1~3 Alkanol, C 1~3 More preferably, the liquid carrier optionally comprises 0 to 20 wt. % (preferably 1 to 17.5 wt. %, more preferably 2.5 to 15 wt. %, and most preferably 5 to 12 wt. %) of a water-miscible liquid, based on the weight of the liquid carrier, the water-miscible liquid comprising ethanol, monoethanolamine, and propylene glycol.

[0025] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention contains cellulase. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention contains 0.001 to 2 wt. % (preferably, 0.01 to 1 wt. %, more preferably, 0.05 to 0.5 wt. %, and most preferably, 0.075 to 0.2 wt. %) of cellulase based on the weight of the aqueous cotton regeneration composition. Most preferably, the aqueous cotton regeneration composition formed by the method of the present invention contains 0.001 to 2 wt. % (preferably, 0.01 to 1 wt. %, more preferably, 0.05 to 0.5 wt. %, and most preferably, 0.075 to 0.2 wt. %) of cellulase based on the weight of the aqueous cotton regeneration composition, the cellulase being of bacterial or fungal origin (preferably, the cellulase may be a chemically or genetically modified variant). Suitable cellulases may include cellulases derived from the genera Bacillus, Pseudomonas, Fusorium, Hamicola, Chelabia, Acremonium, and Myceliophore. Preferred cellulases may include cellulases derived from Humicola insolens, Myceliophthora thermophila, and Fusorium oxysporum. Commercially available cellulases include Carezyme™, Celluzyme™, Celluclean™, Celluclast™, Endolase™, Renozyme™, Whitezyme™ (available from Novozymes A / S), Clazinase™, Puradax, Puradax HA, and Puradax EG (available from Genencor), and KAC-500(B)™ (available from Kao Corporation).

[0026] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises a protectant polymer. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises 0.05 to 5 wt. % (preferably, 0.1 to 3 wt. %, more preferably, 0.25 to 2.0 wt. %, and most preferably, 0.4 to 1 wt. %) of a protectant polymer, based on the weight of the aqueous cotton regeneration composition. Most preferably, the aqueous cotton regeneration composition formed by the method of the present invention comprises 0.05 to 5 wt. % (preferably, 0.1 to 3 wt. %, more preferably, 0.25 to 2.0 wt. %, and most preferably, 0.4 to 1 wt. %) of a protectant polymer, based on the weight of the aqueous cotton regeneration composition, the protectant polymer comprising 25 to 65 wt. % (preferably, 30 to 60 wt. %, more preferably, 35 to 55 wt. %, and most preferably, 40 to 44 wt. %) of structural units of formula I (wherein each R 1 are independently selected from hydrogen and —CH groups) (preferably, 20 to 60 mole % of the structural units of formula I in the protectant polymer are R 1 is hydrogen, and more preferably, 30 to 50 mole percent of the structural units of formula I in the protectant polymer are R 1 is hydrogen, and even more preferably, 35 to 45 mole percent of the structural units of formula I in the protectant polymer are R 1 is hydrogen, and most preferably, 37.5 to 42.5 mole percent of the structural units of formula I in the protectant polymer are R 1 is hydrogen) and 35 to 75 weight percent of structural units of formula II, based on the weight of the protectant polymer, 2 -C 2~3 alkyl groups (preferably -C alkyl groups), and each R 3 are independently selected from hydrogen and methyl groups (preferably hydrogen).

[0027] Preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention comprises 25 to 65 wt. % (preferably, 30 to 60 wt. %, more preferably, 35 to 55 wt. %, and most preferably, 40 to 44 wt. %) of structural units of formula I (wherein each R 1are independently selected from hydrogen and —CH groups). More preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the process of the present invention comprises 25 to 65 wt. % (preferably, 30 to 60 wt. %, more preferably, 35 to 55 wt. %, and most preferably, 40 to 44 wt. % of structural units of formula I, based on the weight of the protectant polymer, where R 1 is hydrogen in 20 to 60 mol % (preferably 30 to 50 mol %, more preferably 35 to 45 mol %, most preferably 37.5 to 42.5 mol %) of the structural units of formula I in the protectant polymer.

[0028] Preferably, the protectant polymer used in the aqueous cotton regenerating composition formed in the process of the present invention comprises 35 to 75 wt. % (preferably, 40 to 70 wt. %, more preferably, 45 to 65 wt. %, and most preferably, 56 to 60 wt. %) of structural units of formula II, based on the weight of the protectant polymer, wherein each R 2 -C 2~3 alkyl groups, and each R 3 are independently selected from hydrogen and methyl groups. More preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the process of the present invention comprises 35 to 75 wt. % (preferably 40 to 70 wt. %, more preferably 45 to 65 wt. %, and most preferably 56 to 60 wt. %) of structural units of formula II, based on the weight of the protectant polymer, wherein each R 2 -C 2~3 independently selected from alkyl groups, R 2 are ethyl groups in 75 to 100 mol % (preferably 90 to 100 mol %, more preferably 98 to 100 mol %, most preferably 100 mol %) of the structural units of formula II in the protectant polymer, 3 are independently selected from hydrogen and a methyl group; R 3is hydrogen at 75 to 100 mol % (preferably 90 to 100 mol %, more preferably 98 to 100 mol %, and most preferably 100 mol %) of the structural units of formula II in the protectant polymer. Most preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention comprises 35 to 75 wt % (preferably 40 to 70 wt %, more preferably 45 to 65 wt %, and most preferably 56 to 60 wt %) of structural units of formula II, based on the weight of the protectant polymer, where R 2 is an ethyl group, and each R 3 is hydrogen.

[0029] Preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention has a weight average molecular weight, M, of 1,200 to 100,000 Daltons. w More preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention has a weight average molecular weight, M w Even more preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention has a weight average molecular weight of 10,000 to 60,000 Daltons, M w Most preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention has a weight average molecular weight, M, of 25,000 to 50,000 Daltons. w It has.

[0030] Preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention comprises ≦0.3 wt. % (more preferably ≦0.1 wt. %, even more preferably ≦0.05 wt. %, even more preferably ≦0.03 wt. %, and most preferably <detectable limit) structural units of a multi-ethylenically unsaturated crosslinking monomer, based on the weight of the protectant polymer.

[0031] Preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the method of the present invention comprises ≦1 wt. % (preferably ≦0.5 wt. %, more preferably ≦0.001 wt. %, even more preferably ≦0.0001 wt. %, and most preferably <detectable limit) of sulfonated monomer structural units, based on the weight of the protectant polymer. More preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the process of the present invention comprises ≦1 wt. % (preferably ≦0.5 wt. %, more preferably ≦0.001 wt. %, even more preferably ≦0.0001 wt. %, more preferably <the limit of detectability) of a sulfonated monomer structural unit selected from the group consisting of 2-acrylamido-2-methylpropane sulfonic acid (AMPS), 2-methacrylamido-2-methylpropane sulfonic acid, 4-styrene sulfonic acid, vinyl sulfonic acid, 3-allyloxysulfonic acid, 2-hydroxy-1-propane sulfonic acid (HAPS), 2-sulfoethyl(meth)acrylic acid, 2-sulfopropyl(meth)acrylic acid, 3-sulfopropyl(meth)acrylic acid, 4-sulfobutyl(meth)acrylic acid, and salts thereof, based on the weight of the protectant polymer. Most preferably, the protectant polymer used in the aqueous cotton regenerating composition formed by the process of the present invention comprises ≦1 wt. % (preferably ≦0.5 wt. %, more preferably ≦0.001 wt. %, even more preferably ≦0.0001 wt. %, most preferably <detectable limit) structural units of 2-acrylamido-2-methylpropanesulfonic acid (AMPS) monomer, based on the weight of the protectant polymer.

[0032] Methods for making the protectant polymers used in the aqueous cotton reclaim compositions formed by the process of the present invention are well known in the art.

[0033] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention contains <1 wt. % (preferably, <0.5 wt. %, more preferably, <0.2 wt. %, even more preferably, <0.1 wt. %, even more preferably, <0.01 wt. %, and most preferably, <detectable limits) vinyl alcohol polymer (PVA), based on the dry weight of the aqueous cotton regeneration composition.

[0034] Preferably, the aqueous cotton regeneration composition formed by the process of the present invention contains <0.1 wt. % (preferably, <0.05 wt. %, more preferably, <0.02 wt. %, even more preferably, <0.01 wt. %, even more preferably, <0.001 wt. %, and most preferably, <the limit of detectability) of a low molecular weight carboxylic acid selected from the group consisting of formate, acetate, propionate, and mixtures thereof, based on the dry weight of the aqueous cotton regeneration composition.

[0035] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention contains <0.1 wt. % (preferably, <0.05 wt. %, more preferably, <0.02 wt. %, even more preferably, <0.01 wt. %, even more preferably, <0.001 wt. %, and most preferably, <the limit of detectability) of boron-containing compounds, based on the dry weight of the aqueous cotton regeneration composition.

[0036] Preferably, the aqueous cotton regeneration composition formed by the process of the present invention contains <0.1 wt. % (preferably, <0.05 wt. %, more preferably, <0.02 wt. %, even more preferably, <0.01 wt. %, even more preferably, <0.001 wt. %, and most preferably, <the limit of detectability) of an alpha-hydroxy-monocarboxylic acid or a salt of an alpha-hydroxy-monocarboxylic acid, based on the dry weight of the aqueous cotton regeneration composition.

[0037] Preferably, the aqueous cotton regenerating composition formed by the method of the present invention optionally further comprises an additional ingredient selected from the group consisting of at least one of a detersive surfactant, a structurant, a hydrotrope, a fragrance, a foam control agent (e.g., fatty acid, polydimethylsiloxane), a builder, and a fabric softener.

[0038] Preferably, the aqueous cotton regenerating composition formed by the process of the present invention is a liquid laundry detergent formulation further comprising a cleaning surfactant. More preferably, the aqueous cotton regenerating composition formed by the process of the present invention is a liquid laundry detergent formulation and comprises 2 to 60 wt. % (more preferably, 5 to 50 wt. %, even more preferably, 7.5 to 40 wt. %, even more preferably, 10 to 30 wt. %, and most preferably, 15 to 25 wt. %) of a cleaning surfactant. Even more preferably, the aqueous cotton regenerating composition formed by the process of the present invention is a liquid laundry detergent formulation and further comprises 2 to 60 wt. % (more preferably, 5 to 50 wt. %, even more preferably, 7.5 to 40 wt. %, even more preferably, 10 to 30 wt. %, and most preferably, 15 to 25 wt. %) of a cleaning surfactant, based on the weight of the liquid laundry detergent formulation, wherein the cleaning surfactant is selected from the group consisting of anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, and mixtures thereof. Even more preferably, the aqueous cotton regenerating composition formed by the process of the present invention is a liquid laundry detergent formulation and further comprises 2 to 60 wt. % (more preferably, 5 to 50 wt. %, even more preferably, 7.5 to 40 wt. %, even more preferably, 10 to 30 wt. %, and most preferably, 15 to 25 wt. %) of a cleaning surfactant, based on the weight of the liquid laundry detergent formulation, wherein the cleaning surfactant is selected from the group consisting of a mixture comprising an anionic surfactant and a nonionic surfactant. Most preferably, the aqueous cotton regenerating composition formed by the process of the present invention is a liquid laundry detergent formulation and further comprises 2 to 60 wt. % (more preferably, 5 to 50 wt. %, even more preferably, 7.5 to 40 wt. %, even more preferably, 10 to 30 wt. %, and most preferably, 15 to 25 wt. %) of a cleaning surfactant, based on the weight of the liquid laundry detergent formulation, wherein the cleaning surfactant comprises a mixture of linear alkyl benzene sulfonate, sodium lauryl ethoxy sulfate, and nonionic alcohol ethoxylate.

[0039] Anionic surfactants include alkyl sulfates, alkylbenzene sulfates, alkylbenzene sulfonic acids, alkylbenzene sulfonates, alkyl polyethoxy sulfates, alkoxylated alcohols, paraffin sulfonic acids, paraffin sulfonates, olefin sulfonic acids, olefin sulfonates, alpha-sulfocarboxylates, esters of alpha-sulfocarboxylates, alkyl glyceryl ether sulfonic acids, alkyl glyceryl ether sulfonates, sulfates of fatty acids, sulfonates of fatty acids, sulfonates of fatty acid esters, alkyl phenols, alkylphenol polyethoxy ether sulfates, 2-acryloxy-alkane-1-sulfonic acids, 2-acryloxy-alkane-1-sulfonates, beta-alkyloxyalkane sulfonic acids, beta-alkyloxyalkane sulfonates, amine oxides, and mixtures thereof. Preferred anionic surfactants include C 8~20 Alkylbenzene sulfate, C 8~20 Alkylbenzene sulfonic acid, C 8~20 Alkylbenzene sulfonates, paraffin sulfonic acids, paraffin sulfonates, alpha-olefin sulfonic acids, alpha-olefin sulfonates, alkoxylated alcohols, C 8~20 Alkylphenols, amine oxides, sulfonates of fatty acids, sulfonates of fatty acid esters, C 8~10 alkyl polyethoxy sulfates, and mixtures thereof. More preferred anionic surfactants include C 12~16 Alkylbenzene sulfonic acid, C 12~16 Alkylbenzene sulfonic acid, C 12~18 Paraffin sulfonic acid, C 12~18 Paraffin sulfonic acid, C 12~16 Alkyl polyethoxy sulfates, and mixtures thereof.

[0040] Nonionic surfactants include alkoxylates, polyglycol ethers, fatty alcohol polyglycol ethers, alkylphenol polyglycol ethers, end-capped polyglycol ethers, mixed ethers, hydroxy mixed ethers, fatty acid polyglycol esters, and mixtures thereof. Preferred nonionic surfactants include alkoxylates. More preferred nonionic surfactants include ethoxylated and propoxylated alcohols. Most preferred nonionic surfactants include ethoxylated and propoxylated alcohols derived from biorenewable seed oil alcohols.

[0041] The cationic surfactant includes a quaternary surface-active compound.Preferred cationic surfactants include a quaternary surface-active compound having at least one of an ammonium group, a sulfonium group, a phosphonium group, an iodonium group, and an arsonium group.More preferred cationic surfactants include at least one of dialkyldimethylammonium chloride and alkyldimethylbenzylammonium chloride.Even more preferred cationic surfactants include C 16~18 Dialkyldimethylammonium chloride, C 8~18 The most preferred cationic surfactants include at least one of alkyldimethylbenzylammonium chloride, ditallowdimethylammonium chloride, and ditallowdimethylammonium chloride.

[0042] Examples of amphoteric surfactants include betaine, amine oxide, alkylamidoalkylamine, alkyl-substituted amine oxide, acylated amino acid, derivatives of aliphatic quaternary ammonium compounds, and mixtures thereof. Preferred amphoteric surfactants include derivatives of aliphatic quaternary ammonium compounds. More preferred amphoteric surfactants include derivatives of aliphatic quaternary ammonium compounds having a long-chain group with 8 to 18 carbon atoms. Even more preferred amphoteric surfactants include C 12~14The most preferred amphoteric surfactants include at least one of alkyl dimethylamine oxide, 3-(N,N-dimethyl-N-hexadecyl-ammonio)propane-1-sulfonate, and 3-(N,N-dimethyl-N-hexadecylamino)-2-hydroxypropane-1-sulfonate. 12~14 At least one of alkyl dimethyl amine oxides may be mentioned.

[0043] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a structuring agent. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention further comprises 0 to 2 wt. % (preferably, 0.05 to 0.8 wt. %, more preferably, 0.1 to 0.4 wt. %) of a structuring agent, based on the weight of the aqueous cotton regeneration composition. Most preferably, the aqueous cotton regeneration composition formed by the method of the present invention further comprises 0 to 2 wt. % (preferably, 0.05 to 0.8 wt. %, more preferably, 0.1 to 0.4 wt. %) of a structuring agent, based on the weight of the aqueous cotton regeneration composition, the structuring agent being a non-polymeric crystalline hydroxy-functional material capable of forming a thread-like structuring system throughout the aqueous cotton regeneration composition when crystallized in situ. The structuring agent is useful for providing sufficient yield stress or low-shear viscosity to stabilize the aqueous cotton regeneration composition.

[0044] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a hydrotrope. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises 0 to 10 wt % (preferably 0.1 to 7.5 wt %, more preferably 0.2 to 5 wt %, and most preferably 0.5 to 2.5 wt %) of a hydrotrope, based on the weight of the aqueous cotton regeneration composition. More preferably, the aqueous cotton regenerating composition formed by the process of the present invention optionally further comprises 0 to 10 wt. % (preferably, 0.1 to 7.5 wt. %, more preferably, 0.2 to 5 wt. %, and most preferably, 0.5 to 2.5 wt. %) of a hydrotrope, based on the weight of the aqueous cotton regenerating composition, the hydrotrope being selected from the group consisting of calcium, sodium, potassium, ammonium, and alkanolammonium salts of alkyl hydroxides, glycols, urea, monoethanolamine, diethanolamine, triethanolamine, xylene sulfonic acid, toluene sulfonic acid, ethylbenzene sulfonic acid, naphthalene sulfonic acid, and cumene sulfonic acid, salts thereof, and mixtures thereof. Most preferably, the aqueous cotton regenerating composition formed by the process of the present invention further comprises 0 to 10 wt. % (preferably, 0.1 to 7.5 wt. %, more preferably, 0.2 to 5 wt. %, and most preferably, 0.5 to 2.5 wt. %) of a hydrotrope, based on the weight of the aqueous cotton regenerating composition, the hydrotrope being selected from the group consisting of sodium toluene sulfonate, potassium toluene sulfonate, sodium xylene sulfonate, ammonium xylene sulfonate, potassium xylene sulfonate, calcium xylene sulfonate, sodium cumene sulfonate, ammonium cumene sulfonate, and mixtures thereof.

[0045] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a fragrance. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises 0 to 10 wt % (preferably 0.001 to 5 wt %, more preferably 0.005 to 3 wt %, and most preferably 0.01 to 2.5 wt %) of a fragrance, based on the weight of the aqueous cotton regeneration composition.

[0046] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a builder. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises 0 to 50 wt % (preferably 5 to 50 wt %, more preferably 7.5 to 30 wt %) of a builder, based on the weight of the aqueous cotton regeneration composition. Most preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises 0 to 50 wt. % (preferably, 5 to 50 wt. %, more preferably, 7.5 to 30 wt. %) of a builder, based on the weight of the aqueous cotton regeneration composition, the builder being selected from the group consisting of inorganic builders (e.g., tripolyphosphate, pyrophosphate), alkali metal carbonates, borates, bicarbonates, hydroxides, zeolites, citrates (e.g., trisodium citrate dihydrate), polycarboxylates, monocarboxylates, aminotrismethylenephosphonic acid, salts of aminotrismethylenephosphonic acid, hydroxyethanediphosphonic acid, salts of hydroxyethanediphosphonic acid, diethylenetriaminepenta(methylenephosphonic acid), salts of diethylenetriaminepenta(methylenephosphonic acid), ethylenediaminetetraethylene-phosphonic acid, salts of ethylenediaminetetraethylene-phosphonic acid, oligomeric phosphonates, polymeric phosphonates, and mixtures thereof.

[0047] Preferably, the aqueous cotton regenerating composition formed by the method of the present invention optionally further comprises a fabric softener. More preferably, the aqueous cotton regenerating composition formed by the method of the present invention optionally further comprises 0 to 10 wt. % (preferably 0.5 to 10 wt. %) of a fabric softener, based on the weight of the aqueous cotton regenerating composition. Most preferably, the aqueous cotton regenerating composition formed by the method of the present invention optionally further comprises 0 to 10 wt. % (preferably 0.5 to 10 wt. %) of a fabric softener, based on the weight of the aqueous cotton regenerating composition, the fabric softener being a cationic coacervated polymer (e.g., cationic hydroxyethyl cellulose, polyquaternium polymer, and combinations thereof).

[0048] Preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a pH adjuster. More preferably, the aqueous cotton regeneration composition formed by the method of the present invention optionally further comprises a pH adjuster, and the aqueous cotton regeneration composition has a pH of 6 to 12.5 (preferably, 6.5 to 11, more preferably, 7.5 to 10). Bases for adjusting pH include mineral bases such as sodium hydroxide (including soda ash) and potassium hydroxide, sodium bicarbonate, sodium silicate, ammonium hydroxide, and organic bases (e.g., mono-, di-, or tri-ethanolamine, and 2-dimethylamino-2-methyl-1-propanol (DMAMP)). Acids for adjusting pH include mineral acids (e.g., hydrochloric acid, phosphoric acid, and sulfuric acid) and organic acids (e.g., acetic acid).

[0049] Preferably, the soiled cotton-containing fabric provided in the method of the present invention is selected from the group consisting of at least one of soiled cotton fabric, soiled polyester-cotton blend fabric, soiled cotton interlock fabric, and soiled cotton terry fabric (preferably, the soiled cotton-containing fabric is soiled with at least one of oil and clay, more preferably, the soiled cotton-containing fabric is soiled with sebum oil and clay). More preferably, the soiled cotton-containing fabric provided in the method of the present invention is selected from the group consisting of at least one of soiled cotton fabric and soiled polyester-cotton blend fabric (preferably, the soiled cotton-containing fabric is soiled with at least one of oil and clay, more preferably, the soiled cotton-containing fabric is soiled with sebum oil and clay).

[0050] Some embodiments of the present invention are described in detail in the following examples.

[0051] The monomer abbreviations used in the examples are explained in Table 1.

[0052] [Table 1]

[0053] Synthetic S1: Protectant Polymer A monomer emulsion was prepared in a plastic-coated container by adding 28% sodium lauryl sulfate (9.4 g) and deionized water (309.3 g) and mixing with an overhead stirrer. Ethyl acrylate (297.2 g) was then charged to the plastic-coated container, followed by methacrylic acid (138.8 g). Acrylic acid (77.11 g) was then slowly added to the contents of the plastic-coated container, forming a smooth, stable monomer emulsion.

[0054] An initiator solution was prepared in a separate container by adding ammonium persulfate (0.55 g) and deionized water (18.6 g).

[0055] A cofeed catalyst solution was prepared in a separate container by dissolving ammonium persulfate (0.22 g) in deionized water (47 g).

[0056] A 3-liter round-bottom flask equipped with a mechanical stirrer, heating mantle, thermocouple, condenser, and inlets for monomer, initiator, and nitrogen addition was charged with deionized water (609 g), followed by 28% sodium lauryl sulfate (13.73 g), followed by deionized water (15 g). The contents of the flask were then set to stir with a nitrogen flow and heated to 89°C. When the contents of the flask reached 89°C, 13.73 g of 28% sodium lauryl sulfate was added, followed by 15 g of deionized water. 41.6 g of the monomer emulsion from a plastic-coated container was then charged to the contents of the flask, followed by the initiator solution. Once the reaction had begun in the flask, 1-dodecanethiol (10 g) was added to the stirred monomer emulsion in the plastic-coated container. The contents of the plastic-coated vessel were then added to the contents of the flask at 8.89 mL / min over 90 minutes, maintaining a temperature of 84-86°C. The feed of the cofeed catalyst solution to the contents of the flask was started simultaneously with the monomer feed from the plastic-coated vessel and continued at a constant rate over 95 minutes. A rinse of deionized water (36 g) was then added to the contents of the flask through the monomer feed line. At the end of the cofeed catalyst solution, the contents of the flask were held at 85°C for 20 minutes.

[0057] A chaser solution of ammonium persulfate (0.22 g) dissolved in 62.6 g of deionized water (62.6 g) was prepared. The chaser solution was added at a rate of 3.15 g / min over 20 minutes while the contents of the flask were cooled to 75° C. The contents of the flask were then held for 15 minutes.

[0058] A chase activator solution was prepared by dissolving 70% tert-butyl hydroperoxide (1.25 g) in deionized water (34.6 g). A catalyst solution was prepared by dissolving isoascorbic acid (1.77 g) in deionized water (42.1 g).

[0059] An accelerator solution of 0.15% iron sulfate heptahydrate solution (2.8 g) was added to the contents of the flask. The chaser activator solution and catalyst solution were then added to the contents of the flask over 45 minutes while the contents of the flask were cooled to 55°C. The contents of the flask were then held for 5 minutes. Deionized water (50 g) was then added to the contents of the flask and cooling was initiated.

[0060] A pH buffer solution of sodium benzoate (2.4 g) dissolved in deionized water (15 g) was prepared. The pH buffer was added to the contents of the flask over 5 minutes when the contents of the flask had cooled to <40° C. The contents of the flask were then further cooled to room temperature and the product emulsion polymer was filtered through a 100 mesh bag.

[0061] The product emulsion polymer had a solids content of 29.1% and a pH of 3.7. Total residual monomer content was <100 ppm by GC.

[0062] Synthetic S2: Protectant Polymer Glacial acrylic acid (AA) feed (356.4 g) was added to a graduated cylinder.

[0063] 2-(dimethylamino) ethyl methacrylate (DMAEMA) feed (39.6 g) was added to the syringe.

[0064] An initiator solution was prepared in a separate container by dissolving sodium persulfate (2.42 g) in deionized water (25 g).

[0065] A chain regulator solution was prepared in a separate container by dissolving 25.64 g of sodium metabisulfite (25.64 g) in 64 g of deionized water (64 g).

[0066] A precharge solution was prepared in a separate container by dissolving sodium metabisulfite (1.08 g) in deionized water (5 g).

[0067] A 0.15% iron sulfate heptahydrate accelerator solution (3.32 g) was prepared in a separate container.

[0068] A 2-liter round-bottom flask equipped with a mechanical stirrer, heating mantle, thermocouple, condenser, and addition ports for monomer, initiator, and chain regulator was charged with deionized water (346 g). The contents of the flask were set to stir and heated to 72°C.

[0069] Once the contents of the flask reached 72°C, the accelerator solution was added, followed by a deionized water rinse (1.4g), followed by the precharge solution. The following feeds to the contents of the flask were started simultaneously: Chain regulator solution - 1.18 g / min, 75 min, Glacial acrylic acid (AA) feed - 3.95 g / min for 90 min 2-(dimethylamino)ethyl methacrylate (DMAEMA) feed—0.44 g / min for 90 min, and Initiator solution - 0.28g / min for 95 min.

[0070] At the completion of these feeds, 6 g of deionized water was added through the glacial acrylic acid (AA) feed line and 6 g of deionized water was added to the contents of the flask through the DMAEMA syringe, and the contents of the flask were then held at 72° C. for 10 minutes.

[0071] A first chase solution was prepared using sodium persulfate (0.99 g) and deionized water (10 g). A second chase solution was prepared using sodium persulfate (1.08 g) and deionized water (10 g).

[0072] At the completion of the 10 minute hold, a first chase solution was added linearly to the contents of the flask over 10 minutes. The contents of the flask were then held at 72°C for 20 minutes. A second chase solution was then added to the contents of the flask over 10 minutes. The contents of the flask were then held at 72°C for 20 minutes.

[0073] At the completion of the final hold, deionized water (51 g) was added to the contents of the flask while cooling. Once the contents of the flask reached <50°C, monoethanolamine (203 g) was added to the addition funnel and slowly added to the contents of the flask over 30 minutes, controlling the exotherm to maintain the contents of the flask below 70°C. The funnel was then rinsed into the contents of the flask with deionized water (8 g). 35% hydrogen peroxide solution (1 g) was added to the contents of the flask. Deionized water (60 g) was then added to the contents of the flask. After cooling, the product emulsion polymer was recovered.

[0074] The final polymer had a solids content of 53.7% (measured in a forced draft oven at 150° C. for 60 minutes). The pH of the solution was 6.11, and the final molecular weight, measured by gel permeation chromatography, was 6,848 Da.

[0075] Comparative Examples C1-C5 and Example 1: Aqueous Liquid Laundry Formulation The aqueous liquid laundry formulations used in the anti-redeposition tests in the subsequent examples had the formulations set forth in Table 2, prepared by standard liquid laundry formulation preparation procedures and using protectant polymers from synthesis S1-S2 with the monomer feed compositions shown in Table 3.

[0076] [Table 2]

[0077] [Table 3]

[0078] Prevention of redeposition The anti-redeposition performance of the aqueous liquid laundry formulations of Comparative Examples C1-C5 and Example 1 was evaluated according to the AISE recommended methodology after preparation (time T0) and after aging in a closed container at 40°C for 7 weeks (time T7-40°C). A washing machine (Novotronic W 1614 from Miele) was used under the conditions shown in Table 4.

[0079] [Table 4]

[0080] The fabrics were washed six consecutive cycles, and the reflectance Y (D65) of each white swatch (cotton, CO, and polyester:cotton blend, PB) was measured with a spectrophotometric colorimeter (Konica Minolta CM2600d). Each white swatch was folded in the same manner, and the Y value was measured at two points on each side of the fabric, with the average values ​​reported in Table 5.

[0081] [Table 5]

Claims

1. 1. A method of making an aqueous cotton regeneration composition for regenerating soiled cotton-containing fabrics, comprising: providing a liquid carrier; Providing cellulase; selecting a protectant polymer, wherein said protectant polymer comprises 25 to 65 weight percent of a compound of Formula I, based on the weight of said protectant polymer; 【Chemistry 1】 (In the formula, each R １ is hydrogen and -CH ３ groups), and 35 to 75 wt. % of structural units of formula II, based on the weight of the protectant polymer. 【Chemistry 2】 (In the formula, each R ２ is -C ２～３ alkyl groups, and each R ３ are independently selected from hydrogen and methyl groups), providing the selected protectant polymer; and combining the liquid carrier, the cellulase, and the selected protectant polymer to form the aqueous cotton regeneration composition, wherein the aqueous cotton regeneration composition further comprises a pH adjuster, and the aqueous cotton regeneration composition has a pH of 7.5 to 12.

5. A method comprising:

2. 10. The method of claim 1, wherein the protectant polymer is selected based on its cellulase protection ability as demonstrated by the anti-redeposition performance of the aqueous cotton regenerating composition after storage in a sealed container at 40°C for 7 weeks.

3. 3. The method of claim 2, further comprising providing an additional ingredient selected from the group consisting of at least one of a detersive surfactant, an organic solvent, a structurant, a hydrotrope, a fragrance, a suds control agent, a builder, and a fabric softener, and combining the additional ingredient with the liquid carrier, the cellulase, and the selected protectant polymer to form the aqueous cotton regenerating composition.

4. 4. The method of claim 3, wherein the additional ingredient provided comprises a cleansing surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, and mixtures thereof.

5. The method of claim 4 wherein the additional component provided comprises an anionic surfactant.

6. The additional component provided is C １２～１６ Alkylbenzene sulfonic acid, C １２～１６ Alkylbenzene sulfonate, C １２～１８ Paraffin-sulfonic acid, C １２～１８ Paraffin-sulfonate, C １２～１６ 6. The method of claim 5, comprising an anionic surfactant selected from the group consisting of alkyl polyethoxy sulfates, and mixtures thereof.

7. 7. The method of claim 6, wherein the additional component provided comprises a hydrotope.

8. The method of claim 7 , wherein the additional component provided comprises a builder.

9. 8. The method of claim 7, wherein the additional ingredients provided include at least one of an organic solvent and a foam control agent.

10. Providing a soiled cotton-containing cloth; Providing wash water; providing rinse water; contacting the soiled cotton-containing fabric with the aqueous cotton regenerating composition and the wash water to provide a regenerated cotton-containing fabric; 10. The method of claim 1, further comprising contacting the reclaimed cotton-containing fabric with the rinse water to rinse away the aqueous cotton reclaim composition.

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