Highly crystalline alpha-1,3-glucan

Abstract

Disclosed herein is a composition comprising insoluble alpha-glucan particles with high crystallinity and small particle size. For example, the alpha-glucan particles may have a crystallinity of at least about 0.65 and / or an average diameter of less than 1 micron. At least 50% of the glycosidic bonds of the insoluble alpha-glucan in the disclosed particles are alpha-1,3 glycosidic bonds. Also disclosed are methods for producing insoluble alpha-glucan particles and their use in various applications and products.

Description

[Technical Field]

[0001] This application claims the benefits of U.S. Provisional Patent Applications No. 62 / 931,242 (filed November 6, 2019), No. 62 / 931,239 (filed November 6, 2019), No. 63 / 035,978 (filed June 8, 2020), and No. 63 / 084,036 (filed September 28, 2020), all of which are incorporated herein by reference in their entirety.

[0002] This invention relates to the field of polysaccharides. For example, this disclosure relates to crystalline alpha-1,3-glucan, a method for producing the same, and the use of this material in various applications. [Background technology]

[0003] Because polysaccharides are desired for a variety of applications, researchers have sought polysaccharides that are biodegradable and can be economically produced from renewablely sourced raw materials. One such polysaccharide is alpha-1,3-glucan, an insoluble glucan polymer characterized by having an alpha-1,3-glycosidic bond. This polymer has been prepared, for example, using a glucosyltransferase enzyme isolated from Streptococcus salivarius (Non-Patent Document 1). Also, for example, Patent Document 1 discloses the preparation of spun fibers from enzymatically produced alpha-1,3-glucan. In addition, various other glucan materials have been studied to develop novel or improved applications. For example, Patent Document 2 discloses the enzymatic synthesis of several insoluble glucans with mixed alpha-1,3 and alpha-1,6 bonds. [Prior art documents] [Patent Documents]

[0004] [Patent Document 1] U.S. Patent No. 7,000,000 [Patent Document 2] U.S. Patent Application Publication No. 2015 / 0232819 [Non-patent literature]

[0005] [Non-Patent Document 1] Simpson et al., Microbiology 141:1451-1460, 1995 [Overview of the Initiative] [Problems that the invention aims to solve]

[0006] Novel forms of insoluble alpha-glucans are desired to enhance the economic value and performance properties of this material in a variety of applications. To address this need, insoluble alpha-1,3-glucans with high crystallinity and controlled particle size are described herein. [Means for solving the problem]

[0007] In one embodiment, the present disclosure relates to a composition comprising insoluble alpha-glucan particles having a crystallinity of at least about 0.65, wherein the insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least 15, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds.

[0008] In another embodiment, the present disclosure relates to a composition comprising insoluble alpha-glucan particles, wherein at least 80% by weight of the particles are in the form of plates, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds, and (i) at least 70% by weight of the insoluble alpha-glucan particles have a diameter of less than 1.0 micron, and / or (ii) 45 to 55% by weight of the insoluble alpha-glucan particles have a diameter of less than 0.35 micron.

[0009] In another embodiment, the present disclosure relates to a method for producing insoluble alpha-glucan particles as specified herein. Such a method comprises (a) providing an insoluble alpha-glucan produced in an enzymatic reaction comprising at least water, sucrose, and a glucosyltransferase enzyme for synthesizing the insoluble alpha-glucan, wherein the insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least about 200, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds; (b) hydrolyzing the insoluble alpha-glucan to insoluble alpha-glucan particles having a DPw of about 35 to about 100, the hydrolysis being carried out under aqueous conditions at a pH of 2.0 or less; and (c) optionally isolating the insoluble alpha-glucan particles produced in step (b). [Brief explanation of the drawing]

[0010] [Figure 1] The molecular weight (DPw) of alpha-1,3-glucan over time during treatment under low pH hydrolysis conditions is shown. The legend indicates that both undried and dried alpha-1,3-glucan enter the hydrolysis reaction at 40 or 80°C. See Example 1. [Figure 2] The degree of crystallinity of hydrolyzed (DPw 50) and unhydrolyzed (DPw approximately 800) alpha-1,3-glucan is shown. See Example 1. [Figure 3-1] Electron micrographs of hydrolyzed (DPw50) (Figures 3B and 3D) and unhydrolyzed (DPw approximately 800) (Figures 3A and 3C) alpha-1,3-glucan are shown. Reference bars (500, 200, or 100 nm) are provided below each micrograph. See Example 1. [Figure 3-2] Continuation of Figure 3-1. [Figure 4]Shows the particle size distribution of hydrolyzed (DPw50) and non-hydrolyzed (DPw about 800) alpha-1,3-glucan in an aqueous dispersion. See Example 1. [Figure 5] Figure 5A shows the viscosity profiles of 5 wt% aqueous dispersions of alpha-1,3-glucan with DPw50 (0.76CI) or alpha-1,3-glucan with DPw about 800 at a neutral pH of 6.4. See Example 2. Figure 5B shows the viscosity profiles of 5 wt% aqueous dispersions of alpha-1,3-glucan (DPw50, 0.76CI) at pH 2.0 or pH 6.4. See Example 2. [Figure 6] Shows an aqueous preparation (room temperature, pH 4.0) initially prepared as a dispersion containing 4 wt% of alpha-1,3-glucan with DPw50 (0.76CI) or DPw about 800 and 14 wt% of vinyl acetate / ethylene (VAE) latex. The DPw50 alpha-1,3-glucan remains dispersed, while the DPw about 800 alpha-1,3-glucan precipitates. See Example 2. [Figure 7] Shows individual layers of either DPw50 (0.76CI) alpha-1,3-glucan (as 28.3 wt% solids in the dispersion) or DPw about 800 alpha-1,3-glucan (as 33.7 wt% solids in the dispersion) on the "X" mark. The dried DPw50 alpha-1,3-glucan was transparent, while the dried DPw about 800 alpha-1,3-glucan was a hazy white. See Example 4. [Figure 8] Shows the viscosity (at 1 s-1) of 10 wt% aqueous preparations (neutral pH) of non-dried or dried alpha-1,3-glucan (DPw50, 0.76CI or DPw about 800). See Example 5. [Figure 9] Shows a SEM image of a dried emulsion in which alpha-1,3-glucan encapsulates a hydrophobic core. White bar (insert), 5 μm. See Example 7. [[ID=​​​ All patent and non-patent literature disclosures cited herein are incorporated herein by reference in their entirety.

[0012] Unless otherwise disclosed, the terms “one (a)” and “one (an)” as used herein are intended to encompass one or more (i.e., at least one) of the features referred to.

[0013] Where applicable, unless otherwise specified, all ranges are inclusive and combinable. For example, if the range "1 to 5" (i.e., 1-5) is given, it should be interpreted as including ranges such as "1-4", "1-3", "1-2", "1-2 and 4-5", "1-3 and 5", etc.

[0014] The terms "alpha-glucan" and "alpha-glucan polymer" are used interchangeably in this specification. Alpha-glucan is a polymer containing glucose monomer units linked together by alpha-glycosidic bonds. In typical embodiments, the alpha-glucans of this specification contain 100% alpha-glycosidic bonds or at least about 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, or 99% alpha-glycosidic bonds. An example of an alpha-glucan polymer of this specification is alpha-1,3-glucan.

[0015] The terms "polyalpha-1,3-glucan," "alpha-1,3-glucan," and "alpha-1,3-glucan polymer" are used herein with the same meaning. Alpha-1,3-glucan is a polymer containing glucose monomer units linked to each other by glycosidic bonds, with at least about 50% of the glycosidic bonds being alpha-1,3. In certain embodiments, alpha-1,3-glucan contains at least 90% or 95% alpha-1,3 glycosidic bonds. Most or all of the other bonds in alpha-1,3-glucan herein are typically alpha-1,6, but some bonds may also be alpha-1,2 and / or alpha-1,4.

[0016] As used herein, the term "copolymer" refers to a polymer comprising at least two distinct alpha-glucans, such as dextran and alpha-1,3-glucan. As used herein, the terms "graft copolymer," "branched copolymer," etc., generally refer to a copolymer comprising a "backbone" (or "main chain") and side chains branching from the backbone. The side chains are structurally distinct from the backbone. An example of a graft copolymer as used herein comprises a dextran backbone (or, for example, a dextran backbone modified with about 1% to 35% alpha-1,2 branching) and a side chain of at least one alpha-1,3-glucan containing at least about 50% alpha-1,3 glycosidic bonds. The alpha-1,3-glucan side chains as used herein may have, for example, the alpha-1,3-glucan bonds and molecular weights disclosed herein. In some embodiments, the non-reducing end of dextran can prime alpha-1,3-glucan synthesis by glucosyltransferase enzymes, so the dextran backbone can have an alpha-1,3-glucan elongation region.

[0017] In some aspects of this specification, the terms “dextran,” “dextran polymer,” “dextran molecule,” etc., refer to water-soluble alpha-glucans containing at least 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, 99%, or 99.5% alpha-1,6 glycosidic bonds (the remainder of the bonds are typically all or mostly alpha-1,3). An enzyme capable of synthesizing dextran from sucrose may be described as “dextrancrase” (EC 2.4.1.5). As used herein, the term “dextranase” (alpha-1,6-glucan-6-glucanohydrolase; EC 3.2.1.11) means an enzyme capable of endohydrolysis of 1,6-alpha-glycosidic bonds.

[0018] The terms "glycosidic linkage," "glycosidic bond," and "bond" are used interchangeably in this specification and refer to covalent bonds that link sugar monomers within sugar compounds (oligosaccharides and / or polysaccharides). As used herein, the term "alpha-1,3-glycosidic bond" refers to a type of covalent bond that links alpha-D-glucose molecules to each other via carbon atoms 1 and 3 on adjacent alpha-D-glucose rings. As used herein, the term "alpha-1,6-glycosidic bond" refers to a covalent bond that links alpha-D-glucose molecules to each other via carbon atoms 1 and 6 on adjacent alpha-D-glucose rings. Glycosidic bonds in glucan polymers as used herein may also be referred to as "glycosidic bonds." In this specification, "alpha-D-glucose" is referred to as "glucose."

[0019] The glycosidic bond profiles of alpha-glucans described herein can be determined using any method known in the art. For example, the bond profile can be determined by nuclear magnetic resonance (NMR) spectroscopy (e.g., 13 13C NMR and / or 1This can be determined using methods employing 1H NMR. These and other methods that can be used are disclosed, for example, in Food Carbohydrates: Chemistry, Physical Properties, and Applications (SWCui, Ed., Chapter 3, SWCui, Structural Analysis of Polysaccharides, Taylor & Francis Group LLC, Boca Raton, FL, 2005), which is incorporated herein by reference.

[0020] The “molecular weight” of alpha-glucan polymers herein may be expressed as weight-average molecular weight (Mw) or number-average molecular weight (Mn), in units of Daltons (Da) or grams / moles. Alternatively, the molecular weight of alpha-glucan polymers may be expressed as DPw (weight-average degree of polymerization) or DPn (number-average degree of polymerization). The molecular weight of smaller alpha-glucan polymers, such as oligosaccharides, may optionally be provided as “DP” (degree of polymerization), which simply refers to the number of glucose molecules contained within the alpha-glucan. “DP” can also characterize the molecular weight of a polymer on an individual molecular basis. Various methods for calculating these various molecular weights are known in the art, such as high-pressure liquid chromatography (HPLC), size exclusion chromatography (SEC), or gel permeation chromatography (GPC).

[0021] As used herein, Mw is defined as Mw = ΣNiMi 2The molecular weight (Mw) of a polymer can be calculated as Mn = ΣNiMi / ΣNi (wherein Mi is the molecular weight of individual chain i, and Ni is the number of chains of that molecular weight). In addition to SEC, the Mw of a polymer can be determined by other techniques such as static light scattering, mass spectrometry, MALDI-TOF (matrix-assisted laser desorption / ionization time-of-flight), small-angle or neutron X-ray scattering, or ultracentrifugation. As used herein, Mn can be calculated as Mn = ΣNiMi / ΣNi (wherein Mi is the molecular weight of chain i, and Ni is the number of chains of that molecular weight). In addition to SEC, the Mn of a polymer can be determined by various colligative methods, such as vapor pressure osmotic pressure measurement, spectroscopic analysis methods, such as proton NMR, proton FTIR, or UV-Vis terminal group determination. As used herein, DPn and DPw can be calculated from Mw and Mn, respectively, by dividing them by the molar mass M1 of a single monomer unit. For unsubstituted glucan polymers, M1 = 162. In the case of substituted (derivative) glucan polymers, M1 = 162 + M f ×DoS, and here, M f is the molar mass of the substituent, and DoS is the degree of substitution (average number of substituents per glucose unit of the glucan polymer).

[0022] The terms “crystalline,” “crystalline solid,” “crystal,” and similar terms refer, as used herein, to solid materials whose constituent elements are arranged in a regularly ordered structure, forming a lattice; such materials are typically part of a larger composition having crystalline and amorphous regions. “Amorphous” materials are amorphous in that their constituent elements are not organized in a fixed lattice pattern, but rather randomly. Crystalline materials that are not amorphous usually have characteristic geometric shapes (e.g., plates). The terms “crystallinity,” “crystallinity index” (CI), “degree of crystallinity,” etc., refer, as used herein, to the fraction (mass fraction or volume fraction) of crystalline insoluble alpha-glucan, which can be expressed in decimal or percentage form (e.g., a crystallinity of 0.65 corresponds to a crystallinity of 65%). This fraction is the total amount or volume including the amorphous content of insoluble alpha-glucan. The crystallinity described herein can be measured using techniques such as differential scanning calorimetry (DSC), X-ray diffraction (XRD), small-angle X-ray scattering (SAXS), infrared spectroscopy and / or density measurement, for example, in accordance with Struszczyk et al. (1987) J.Bacterial.Polym.Sci.33:177-189), U.S. Patent Application Publication No. 2015 / 0247176, No. 2010 / 0233773, or No. 2015 / 0152196, or International Publication No. 2018 / 081263 (all of which are incorporated herein by reference). In some embodiments, the crystallinity of insoluble alpha-1,3-glucan can be determined herein by following methodologies disclosed in the following examples.

[0023] The terms “particle,” “microparticle,” and similar terms are used interchangeably herein and refer to the smallest recognizable unit of a microparticle system. In some embodiments, particles of insoluble alpha-glucan have an average diameter of about 0.05 to 1.0 micrometers. The terms “micronized” and similar terms may be used to characterize particles of insoluble alpha-glucan herein, and micronized insoluble alpha-glucan in typical embodiments of this disclosure is such that the material exists when dispersed under aqueous conditions. In some embodiments, particle size may mean particle diameter and / or the length of the longest particle dimension. Average diameter may be based on the average of the diameters and / or longest particle dimensions of, for example, at least 50, 100, 500, 1000, 2500, 5000, or 10000 or more particles. Particles may, for example, be in plate form.

[0024] The terms “plate,” “plate-like,” “plate-like,” “flake-like,” and similar terms characterize the shape of insoluble alpha-glucan particles in several embodiments. Particles having this shape are generally flat (two-dimensional, not three-dimensional), in contrast to spherical, cylindrical, fibrous, fibrous, rod-like, cubic, needle-like, spongy / porous, plate-like, or several other shapes. Examples of plate shapes relating to particles as used herein are shown in Figures 3B and 3D. Particles as used herein may optionally be referred to as “plate,” “platelet,” and similar terms, and / or collectively as “microcrystalline glucan” and similar terms.

[0025] As used herein, the term "sucrose" refers to a non-reducing disaccharide composed of alpha-D-glucose and beta-D-fructose molecules linked by an alpha-1,2-glycosidic bond. Sucrose is commonly known as sugar. Alternatively, sucrose may be called "alpha-D-glucopyranosyl-(1→2)-beta-D-fructofuranosyl." "Alpha-D-glucopyranosyl" and "glucosyl" are used interchangeably as used herein.

[0026] The terms "glucosyltransferase," "glucosyltransferase enzyme," "GTF," and "glucansucrose" are used interchangeably in this specification. The activity of the glucosyltransferases described herein catalyzes the reaction of the substrate sucrose to produce the products alpha-glucan and fructose. Other products (by-products) of the GTF reaction include glucose, various soluble gluco-oligosaccharides, and leucrose. The wild-type form of the glucosyltransferase enzyme generally contains a signal peptide (which is typically removed by a cleavage process), a variable domain, a catalytic domain, and a glucan-binding domain (from N-terminus to C-terminus). The glucosyltransferases described herein are classified under the glycoside hydrolase family 70 (GH70) according to the CAZy (Carbohydrate-Active EnZymes) database (Cantarel et al., Nucleic Acids Res. 37:D233-238, 2009).

[0027] In this specification, the term "glucosyltransferase catalytic domain" refers to the domain of a glucosyltransferase enzyme that confers alpha-glucan synthesis activity to the glucosyltransferase enzyme. The glucosyltransferase catalytic domain typically does not require the presence of any other domains that possess this activity.

[0028] The terms “enzyme reaction,” “glucosyltransferase reaction,” “glucan synthesis reaction,” “reaction composition,” and “reaction formulation” are used interchangeably in this specification and typically refer to a reaction that initially includes water, sucrose, at least one active glucosyltransferase enzyme, and optionally other components. Components that may be further present in the glucosyltransferase reaction after the glucosyltransferase reaction has usually commenced include fructose, glucose, leucrose, soluble gluco-oligosaccharides (e.g., DP2-DP7) (these may be considered products or by-products depending on the glucosyltransferase used) and / or insoluble alpha-glucan products with a DP of 8 or higher (e.g., DP100 or higher). It will be understood that certain glucan products, such as alpha-1,3-glucan with a degree of polymerization (DP) of at least 8 or 9, are insoluble in water and therefore may not dissolve in the glucan synthesis reaction, but rather exist outside the solution (e.g., due to precipitation from the reaction). This occurs during a glucan synthesis reaction in which water, sucrose, and a glucosyltransferase enzyme are brought into contact. As used herein, “suitable reaction conditions” refers to reaction conditions that facilitate the conversion of sucrose to alpha-glucan products by glucosyltransferase enzyme activity. During such a reaction, the glucosyl groups originally derived from the sucrose are enzymatically transferred and used for alpha-glucan polymer synthesis. Therefore, the glucosyl groups involved in this process may optionally be described as glucosyl components or parts (or similar terms) of the glucosyltransferase reaction. The insoluble alpha-glucans produced by the glycosyltransferase reaction herein can then be used to prepare further insoluble alpha-glucans of the present disclosure, for example, by a hydrolysis procedure.

[0029] In some aspects of this specification, the "yield" of the insoluble alpha-glucan product in a glucosyltransferase reaction represents the molar yield based on the converted sucrose. The molar yield of the alpha-glucan product can be calculated based on the moles of the insoluble alpha-glucan product divided by the moles of the converted sucrose. The moles of converted sucrose can be calculated as follows: (mass of initial sucrose - mass of final sucrose) / molecular weight of sucrose [342 g / mol]. This molar yield calculation can be considered a measure of the selectivity of the reaction for insoluble alpha-glucan. In some aspects, the "yield" of the insoluble alpha-glucan product in a glucosyltransferase reaction can be based on the glucosyl component of the reaction. Such a yield (glucosyl-based yield) can be evaluated using the following formula: Insoluble alpha-glucan yield = ((IS / 2 - (FS / 2 + LE / 2 + GL + SO)) / (IS / 2 - FS / 2)) × 100%.

[0030] The fructose residue from the glucosyltransferase reaction can be evaluated to ensure, where applicable, that the HPLC data is within the acceptable range (90-110% is considered acceptable). The fructose residue can be evaluated using the following formula: Fructose residue = ((180 / 342 × (FS + LE) + FR) / (180 / 342 × IS)) × 100%.

[0031] In the two equations above, IS is [initial sucrose], FS is [final sucrose], LE is [leucrose], GL is [glucose], SO is [soluble oligomer] (gluco-oligosaccharide), and FR is [fructose] (the concentrations of each substrate / product shown in double parentheses are in grams / liter, and are the concentrations measured, for example, by HPLC).

[0032] In this specification, "cake" of insoluble alpha-glucan refers to a preparation in a condensed, compressed, packed, pressed and / or compressed form, comprising at least (i) about 50% to 90% by weight of water or aqueous solution, and (ii) about 10% to 50% by weight of insoluble alpha-glucan. In some embodiments, the cake may also be referred to as "filtered cake" or "wet cake." The cakes described herein typically have a soft, solid-like consistency.

[0033] In this specification, compositions containing “dried” or “to be dried” insoluble alpha-glucan typically contain less than 6, 5, 4, 3, 2, 1, 0.5, or 0.1% by weight of water.

[0034] The term "hydrolysis" and similar terms, as used herein, refer to the decomposition of insoluble alpha-glucans to smaller (lower molecular weight) but still insoluble alpha-glucans, where water is consumed in the cleavage of the glycosidic bonds of the insoluble alpha-glucans. The terms "hydrolysis reaction," "hydrolysis reaction composition," etc., as used herein, typically refer to a reaction that initially comprises at least an aqueous liquid, an insoluble alpha-glucan, and a hydrolyzing agent (e.g., chemical, catalyst / enzyme). Acid hydrolysis reactions described herein include an acid as the hydrolyzing agent, and the pH of the acid hydrolysis reaction may, as used herein, be, for example, 4.0 or less.

[0035] The terms "percent by volume," "volume percentage," "volume%," and "v / v%" are used interchangeably in this specification. The volume percentage of solute in a solution can be calculated using the following formula: [(volume of solute) / (volume of solution)] × 100%.

[0036] The terms "percent by weight," "percent by weight (wt%)," and "percent by weight (%w / w)" are used interchangeably in this specification. Percent by weight refers to the percentage of a substance by mass when the substance is present in a composition, mixture, or solution.

[0037] The terms "weight," "weight / volume percentage," and "w / v%" are used interchangeably in this specification. Weight / volume percentage can be calculated as follows: ((mass of material [g]) / (total volume of material + liquid containing the material [mL])) × 100%. The material may be insoluble in the liquid (i.e., a solid phase in the liquid phase, e.g., a dispersion) or soluble in the liquid (i.e., a solute dissolved in the liquid).

[0038] The term “Pigment Volume Concentration” (PVC) as used herein refers to the ratio of the volume of pigment to the total volume of non-volatile materials present in a coating, and is typically expressed as a percentage. The formula for calculating PVC is as follows: ((Pigment Volume) / (Pigment Volume + Binder Volume + Other Solid Volume)) × 100. “Pigment” as used herein can refer to any organic and / or inorganic entity whose solubility in water is less than 0.01% by weight (e.g., less than 0.0001% by weight) at 20°C and which exhibits light absorption (e.g., absorption with one maximum) at wavelengths in the range of 350 nm to 700 nm.

[0039] The terms “aqueous liquid,” “aqueous fluid,” “aqueous conditions,” “aqueous reaction conditions,” “aqueous setting,” and “aqueous system,” as used herein, may refer to water or aqueous solutions. “Aqueous solution” as used herein may contain one or more dissolved salts, and the maximum total salt concentration may be about 3.5% by weight in some embodiments. While aqueous liquids as used herein typically contain water as the sole solvent in the liquid, aqueous liquids may optionally contain one or more other solvents (e.g., polar organic solvents) that are miscible with water. Thus, an aqueous solution may contain a solvent having at least about 10% by weight of water.

[0040] The “aqueous composition” as used herein has a liquid component comprising, for example, about or at least about 10, 20, 30, 40, 50, 60, 70, 80, 90, 95, 99, or 100% by weight of water. Examples of aqueous compositions include mixtures, solutions, dispersions (e.g., colloidal dispersions), suspensions, and emulsions.

[0041] As used herein, the term “colloidal dispersion” refers to a heterogeneous system having a dispersion phase and a dispersion medium, i.e., microscopically dispersed insoluble particles suspended in an aqueous composition, such as water or an aqueous solution. An example of a colloidal dispersion as used herein is a hydrophilic colloid. All or some of the particles in a colloidal dispersion, such as a hydrophilic colloid, may include the insoluble alpha-1,3-glucan disclosed herein. The terms “dispersant” and “dispersion agent” are used interchangeably herein to refer to a substance that facilitates the formation and / or stabilization of a dispersion system. As used herein, “dispersion” refers to the act of preparing a dispersion of materials in an aqueous liquid. As used herein, the term “latex” (and similar terms) refers to a dispersion of one or more polymer particles in water or an aqueous solution, typically in which at least insoluble alpha-glucan particles are present in the latex composition as dispersed polymer components. In some embodiments, the latex is an emulsion comprising a dispersion of at least insoluble alpha-glucan particles. “Emulsion” as used herein is a dispersion of microdroplets of one liquid in another liquid in which the droplets are insoluble or incompatible (e.g., non-polar substances such as oil or other organic liquids such as alkanes in a polar liquid such as water or aqueous solutions). The emulsion may further comprise dispersed alpha-glucan particles that can optionally stabilize the emulsion, for example. However, in some embodiments, the emulsion may be a “dry emulsion” as used herein. Dry emulsions are typically produced by removing all or most (e.g., >95%, >99%, or >99.5%) of the water in a liquid emulsion by means of freeze-drying or spray-drying.

[0042] For example, the insoluble alpha-glucan particles of the present disclosure can provide stability to a dispersion or emulsion. The “stability” (or “quality of being stable”) of a dispersion or emulsion is, as used herein, the ability of dispersed particles in a dispersion or liquid droplets dispersed in another liquid (emulsion) to remain dispersed for a period of about or at least about 2, 4, 6, 9, 12, 18, 24, 30, or 36 months after the initial preparation of the dispersion or emulsion (for example, about or at least about 70, 75, 80, 85, 90, 95, 96, 97, 98, 99, or 100% by weight of the particles in the dispersion or liquid droplets in the emulsion to remain dispersed). A stable dispersion or emulsion can resist overall creaming, precipitation, aggregation, and / or aggregation of the dispersed / emulsified material.

[0043] Alpha-glucans that are "insoluble," "aqueous-insoluble," or "water-insoluble" (and similar terms) (e.g., alpha-1,3-glucans having a DP of 8 or more) are, as used herein, insoluble (or not recognizably soluble) in water or other aqueous conditions (where the aqueous conditions are optionally further characterized by having a pH of 0 to 9 (e.g., pH 6 to 8) and / or a temperature of about 1 to 130°C (e.g., 20 to 25°C)). In some embodiments, less than 1.0 gram (e.g., an undetectable amount) of a water-insoluble graft copolymer or derivative thereof dissolves in 1000 milliliters of such aqueous conditions (e.g., water at 23°C). In contrast, glucans such as certain oligosaccharides as used herein (e.g., alpha-1,3-glucans having a DP of less than 8) that are "soluble," "aqueous-soluble," or "water-soluble" are recognizably soluble under these conditions.

[0044] As used herein, the term "viscosity" refers to a measure of the degree to which a fluid (aqueous or non-aqueous) resists forces that tend to cause flow. Various units of viscosity that may be used herein include, for example, centipoise (cP, cps) and pascal-second (Pa·s). One centipoise is equal to 1 / 100 poise, and one poise is equal to 0.100 kg·m. -1 ·s -1 It is equal to.

[0045] In this specification, terms such as “crosslinking” and “crosslinked” refer to one or more bonds (typically covalent bonds) that link polymers, such as insoluble alpha-glucan particles disclosed herein. Crosslinks having multiple bonds typically include one or more atoms that are part of the crosslinking agent used to form the crosslinks. In this specification, terms such as “crosslinking agent” and “crosslinking agent” refer to atoms or compounds that can form crosslinks. In this specification, terms such as “crosslinking reaction” and similar terms (e.g., “crosslinked composition,” “crosslinking preparation”) typically refer to a reaction that includes at least a solvent, a crosslinking agent, insoluble alpha-glucan particles and optionally another polymer, the reaction may relate to, for example, the preparation of a film or coating. In some embodiments, the crosslinking reaction includes an aqueous solvent such as water, but in other embodiments, the solvent is non-aqueous.

[0046] The terms "household care products" and "home care" typically refer to products, goods, and services related to the handling, cleaning, maintenance, and / or adjustment of household items. Examples of such products include chemicals, compositions, products, or combinations thereof intended for such care.

[0047] In some embodiments, the terms "fiber" (single), "fiber" (plural), etc., refer herein to staple fibers (staple-length fibers) and continuous fibers. Fibers herein may include alpha-1,3-glucan, natural fibers (e.g., cellulose, cotton, wool, silk), or synthetic fibers (e.g., polyester), or any other type of material disclosed herein that can form fibers.

[0048] The terms “textile,” “fabric,” and “cloth” are used herein with the same meaning to refer to woven materials having a network structure of natural and / or synthetic fibers. Such fibers may be, for example, in the form of twisted yarn or knitted yarn.

[0049] The terms “nonwoven fabric,” “nonwoven product,” and “nonwoven web” refer, as used herein, to a web of individual fibers or filaments interposed in a typically random or undefinable manner. This is in contrast to knitted or woven fabrics, which have a definable network of fibers or filaments. In some embodiments, a nonwoven product includes a nonwoven web bonded or attached to another material, such as a substrate or backing. In some embodiments, a nonwoven fabric may further contain a binder or adhesive (reinforcement agent) that binds adjacent nonwoven fibers together. The nonwoven binder or adhesive can be applied to the nonwoven fabric, for example, in the form of a dispersion / latex, a solution, or a solid, and the treated nonwoven fabric is typically dried.

[0050] The terms “textile care composition,” “laundry care composition,” and similar terms refer, in some forms, to any composition suitable for treating textiles, nonwovens, and / or any similar material. Examples of such compositions include laundry detergents and fabric softeners.

[0051] As used herein, “detergent composition” typically comprises at least one surfactant (detergent compound) and / or one builder. As used herein, “surfactant” refers to a substance that has a tendency to reduce the surface tension of a liquid in which it is dissolved. Surfactants can function, for example, as detergents, wetting agents, emulsifiers, foaming agents and / or dispersants.

[0052] The term "personal care products" and similar terms typically refer to products, goods, and services related to the treatment, cleansing, washing, care, or conditioning of humans. Examples of such products include chemicals, compositions, products, or combinations thereof intended for such care.

[0053] The terms “ingestable product” and “ingestable composition” mean any substance that can be taken orally (i.e., by mouth), either alone or in combination with other substances, whether or not it is intended for consumption. Therefore, ingestible products include foods / beverages. “Food / beverage” means any edible product, such as a solid, semi-solid, or liquid, that is intended for consumption by a human or animal (e.g., for nutritional purposes). For example, “food” may optionally mean “foodstuffs,” “food products,” or other similar terms as used herein. “Non-edible product” (“non-edible composition”) means any composition that can be taken orally for purposes other than the consumption of food or beverages. Examples of non-edible products as used herein include supplements, dietary supplements, functional foods, pharmaceuticals, oral care products (e.g., toothpaste, mouthwash), and cosmetics (e.g., sweetened lip balm). “Pharmaceutical product,” “medicine,” “drug,” or similar terms mean as used herein a composition used to treat a disease or injury and may be administered enterally or parenterally.

[0054] The terms “film,” “sheet,” and similar terms used herein refer to thin, visually continuous materials. A film may be composed as a layer or coating on a material, or it may be standalone (e.g., not adhering to the material surface; self-supporting). As used herein, “coating” (and similar terms) refers to a thin layer covering a material surface. The term “uniform thickness,” used to characterize a film or coating as described herein, may refer to a continuous region where (i) at least 20% of the entire area of ​​the film / coating, and (ii) the standard deviation of the thickness is, for example, less than about 50 nm. The term “continuous layer” means a layer of a composition applied to at least a portion of a substrate, wherein the dry layer of the composition covers 99% or more of the surface to which it is applied, and within the layer, there are less than 1% pores that expose the substrate surface. 99% or more of the surface to which the layer is applied excludes any area of ​​the substrate to which the layer is not applied. Coatings can be manufactured in several embodiments herein. Coating composition (and similar terms) refers to all solid components that form a layer on a substrate, such as the insoluble alpha-glucan particles specified herein, and optionally on pigments, surfactants, dispersants, binders, crosslinking agents and / or other additives.

[0055] The term “paint” (and similar terms) herein refers to a type of coating composition which is a dispersion of pigments in a suitable liquid (e.g., an aqueous liquid) that can be used to form an adhesive coating when spread over a thin coat surface. Paints applied to a surface can provide the surface with color / decoration, protection and / or treatment (e.g., a primer). Paints may optionally be characterized herein as a latex or latex paint by further comprising dispersed insoluble alpha-1,3-glucan (i.e., dispersed polymer).

[0056] "Composite" as used herein comprises two or more components, including insoluble alpha-glucan particles. Typically, the components of a composite are resistant to separation, and one or more components exhibit enhanced and / or different properties compared to the properties of the composite alone (i.e., a composite is not simply a mixture that is easily separable into its first component). Composites are generally solid materials as used herein and can be manufactured, for example, by extrusion or molding processes.

[0057] The terms “sequence identity,” “identity,” and others used herein with respect to polypeptide amino acid sequences (for example, of glucosyltransferases) are defined and determined in U.S. Patent Application Publication No. 2017 / 0002336 (incorporated herein by reference).

[0058] The term “isolated” means a substance (or process) in a form or environment that does not exist in nature. Non-limiting examples of isolated substances include any non-natural substances, such as several forms of the insoluble alpha-1,3-glucan disclosed herein (as well as the enzymatic reactions and other processes used to prepare them). The embodiments disclosed herein are considered to be synthetic / artifacts (impossible to produce without human intervention / involvement) and / or possess properties not found in nature.

[0059] As used herein, the term "increased" can refer to an amount or activity that is at least about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 50%, 100%, or 200% greater than the amount or activity being compared. The terms "increased," "enhanced," "enhanced," "greater," and "improved" are used interchangeably herein.

[0060] Novel forms of insoluble alpha-glucan are desired to enhance the economic value and performance properties of this material in a variety of applications. Compositions containing insoluble alpha-1,3-glucan having high crystallinity and controlled particle size are disclosed herein to address this need.

[0061] Some embodiments of the present disclosure relate to compositions comprising insoluble alpha-glucan particles having a crystallinity of at least about 0.65, wherein the insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least 15, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds. Some other embodiments of the present disclosure relate to compositions comprising insoluble alpha-glucan particles, wherein at least about 70% by weight of the particles are plate-shaped, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds, and (i) at least 80% by weight of the insoluble alpha-glucan particles have a diameter of less than 1.0 micron, and / or (ii) 40-60% by weight of the insoluble alpha-glucan particles have a diameter of less than 0.35 micron. The insoluble alpha-glucan particles disclosed herein have several advantageous characteristics, for example, in some embodiments they are stable under low pH conditions (e.g., stability of molecular weight and / or viscosity of aqueous dispersions of particles), have unique optical properties (e.g., high optical transparency, translucency), have an enhanced viscosity profile (e.g., higher viscosity compared to higher DPw insoluble alpha-glucans, retaining viscosity capacity after drying), and / or have enhanced pigment extender function in paints.

[0062] Typically, at least about 50% of the glycosidic bonds of the insoluble alpha-glucans of the compositions of this disclosure are alpha-1,3 glycosidic bonds. In some embodiments, the insoluble alpha-glucans may contain about or at least about 40%, 50%, 60%, 70%, 80%, 85%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, 99.5%, or 100% of alpha-1,3 glycosidic bonds. Thus, in some embodiments, the insoluble alpha-glucans may have about 60%, 50%, 40%, 30%, 20%, 15%, 10%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1%, 0.5%, or less than 0% of glycosidic bonds that are not alpha-1,3. Generally, non-alpha-1,3 glycosidic bonds are almost entirely or entirely alpha-1,6. In certain embodiments, insoluble alpha-glucans have no branching points, or have about 5%, 4%, 3%, 2%, or less than 1% branching points as a percentage of glycosidic bonds within the glucan. In embodiments in which the alpha-glucan contains 50% alpha-1,3 glycosidic bonds, such glucans do not contain alternans (alternating alpha-1,3 and alpha-1,6 bonds).

[0063] In some embodiments, the DPw or DPn of the insoluble alpha-glucan is at least about 15. In some embodiments, the DPw or DPn of the insoluble alpha-glucan is, for example, about or at least about 15, 20, 25, 30, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 65, 70, 75, 80, 85, 90, 95, 100, 110, 125, 15 It may be 0, 175, 200, 15-100, 25-100, 35-100, 15-80, 25-80, 35-80, 15-60, 25-60, 35-60, 15-55, 25-55, 25-50, 35-55, 35-50, 35-45, 35-40, 40-100, 40-80, 40-60, 40-55, 40-50, 45-60, 45-55 or 45-50% by weight or less.

[0064] In some aspects of this disclosure, the insoluble alpha-glucan particles have a crystallinity (crystallinity index) of at least about 0.65. The degree of crystallinity of the particles is, for example, about or at least about 0.55, 0.60, 0.65, 0.66, 0.67, 0.68, 0.69, 0.70, 0.71, 0.72, 0.73, 0.74, 0.75, 0.76, 0.77, 0.78, 0.79, 0.80, 0.81, 0.82, 0.83, 0.84, 0.85, 0.60~0.83, 0.6 The crystallinity values ​​may be 5-0.83, 0.67-0.83, 0.69-0.83, 0.60-0.81, 0.65-0.81, 0.67-0.81, 0.69-0.81, 0.60-0.78, 0.65-0.78, 0.67-0.78, 0.69-0.78, 0.60-0.76, 0.65-0.76, 0.67-0.76, or 0.69-0.76. Generally, the non-crystalline portion of the insoluble alpha-glucan specified herein is amorphous. From the crystallinity values ​​above, the weight % of amorphous particles is, for example, about or about 45%, 40%, 35%, 30%, 25%, 20%, or less than 15%. The crystallinity of alpha-glucan particles as described herein may be measured by any suitable method (e.g., those listed in the above or below examples), for example: A sample of the insoluble alpha-glucan described herein is dried in a vacuum oven set to about 55-65°C (e.g., 60°C) for at least about 2 hours (e.g., 8-12 hours). The sample is then placed in a stainless steel holder having a well approximately 1-2 cm wide × 3-5 cm long × 3-5 cm deep, and the holder is then loaded into a suitable diffractometer (e.g., X'PERT MPD POWDER diffractometer, PANalytical BV, The Netherlands) set to reflection mode, and the X-ray diffraction pattern of the sample is measured. The X-ray source is a Cu X-ray tube source with an optical focusing mirror and a narrow slit of about 1 / 16°. The X-rays are detected using a 1-D detector and a scattering prevention slit set to about 1 / 8°. Data is collected in a range of 2θ, approximately 4 to 60°, with a step of about 0.1°.Subsequently, a linear baseline from approximately 7.2 to 30.5° is subtracted, and the XRD pattern of a known amorphous alpha-1,3-glucan sample scaled to fit the data is subtracted. Then, the remaining crystalline peaks in that range are fitted using a series of Gaussian curves corresponding to the reflections of known dehydrated alpha-1,3-glucan crystals to analyze the resulting X-ray pattern. The crystallinity index is then obtained by dividing the area corresponding to the crystalline peaks by the total area under the curve from which the baseline was subtracted.

[0065] For example, at least about 80% by weight of the insoluble alpha-glucan particles in the compositions herein are in the form of plates. In some embodiments, about or at least about 60, 65, 70, 75, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, 60-85, 60-80, 60-75, 60-70, 65-85, 65-80, 65-75, 65-70, 70-85, 70-80, or 70-75% by weight of the insoluble alpha-1,3-glucan particles are in the form of plates. The plates of insoluble alpha-1,3-glucan of the present invention may be visually identical or similar to the particles shown in Figures 3B and 3D (when observed by electron microscopy, such as TEM or SEM). Typically, the remainder of insoluble alpha-glucan particles in the composition is in a non-plate form, such as that shown in Figure 3C. In some embodiments, the remainder of particles that are in a non-plate form can be characterized as having a fibrous and / or linear appearance. However, in some embodiments, about or at least about 10, 20, 30, 40, 50, 60, or 70% by weight of the insoluble alpha-glucan particles in the compositions herein are in a plate form.

[0066] In some embodiments of the present disclosure, at least about 70% by weight of the insoluble alpha-glucan particles of the composition have a diameter of less than 1.0 micron. In some further embodiments, about or at least about 65% by weight, 70% by weight, 75% by weight, 80% by weight, 85% by weight, 90% by weight, 95% by weight, 65-95% by weight, 70-95% by weight, 75-95% by weight, 80-95% by weight, 85-95% by weight, 65-90% by weight, 70-90% by weight, 75-90% by weight, 80-90% by weight, 85-90% by weight, 65-85% by weight, 70-85% by weight, 75-85% or 80-85% by weight of the insoluble alpha-glucan particles of the composition have a diameter of less than 1.0 micron. In some embodiments, approximately 40-60% by weight, 40-55% by weight, 45-60% by weight, 45-55% by weight, 47-53% by weight, 48-52% by weight, 49-51% by weight, or 50% by weight of insoluble alpha-glucan particles are approximately 1.0, 0.9, 0.8, 0.7, 0.6, 0.5, 0.4, 0.35, 0.34, 0.32, 0.30, 0.28, 0.26, 0.25, 0.24, 0.23, 0.22, 0.21, 0.20, They have diameters of 0.19, 0.18, 0.17, 0.16, 0.15, 0.14, 0.13, 0.12, 0.11, 0.10, 0.10-1.0, 0.10-0.80, 0.10-0.60, 0.10-0.40, 0.10-0.35, 0.10-0.30, 0.10-0.25, 0.10-0.20, 0.15-0.35, 0.15-0.30, 0.15-0.25, or 0.15-0.20 microns or less. These micron values ​​can optionally be considered as "D50" (diameter-50) values. In some embodiments, the alpha-glucan particles have a thickness of approximately 0.010, 0.015, 0.020, 0.025, 0.030, or 0.010-0.030 microns, and such thicknesses can be combined with any of the above diameter embodiments.Particle size can be measured, as described herein, for example, in any of U.S. Patent No. 6,091,492, No. 6,741,350, and No. 9,297,737 (all incorporated herein by reference), and / or as disclosed in the following examples, by processes involving light scattering or changes in electrical impedance (e.g., using a Coulter Counter). Particle size and / or distribution can be measured with respect to particles contained in an aqueous dispersion and / or can be measured using, for example, light scattering techniques.

[0067] In some aspects, alpha-glucan particles have a polydispersity index (PDI) of approximately or less than 1.13, 1.17, 1.2, 1.23, 1.27, 1.3, 1.13–1.3, 1.13–1.27, 1.13–1.23, 1.17–1.3, 1.17–1.27, 1.17–1.23, or 1.18–1.22.

[0068] The alpha-glucans described herein are insoluble in aqueous systems that are not highly alkaline, for example, systems with a pH ≤ 10 or 11. Generally, the solubility of glucan polymers in aqueous systems described herein is related to their bond profile, molecular weight, and / or degree of branching. For example, alpha-1,3-glucans with ≥ 95% 1,3 bonds are generally insoluble under aqueous conditions at 20°C with a DP of 8 or higher. Generally, as the molecular weight increases, the proportion of alpha-1,3 bonds required for the insolubility of alpha-1,3-glucans decreases.

[0069] The insoluble alpha-glucan particles described herein can be prepared, for example, by the hydrolysis methods disclosed herein. Typically, the insoluble alpha-glucan particles and / or any precursor thereof described herein do not undergo any chemical derivatization (e.g., etherification, esterification, phosphorylation, sulfation) (e.g., there is no hydrogen substitution of the glucan hydroxyl group by a non-sugar chemical group). The insoluble alpha-glucans used for the preparation of the particles described herein are typically enzymatically induced in an inert container (typically under cell-free conditions) and are not derived from cell walls (e.g., fungal cell walls).

[0070] Some embodiments of the present disclosure relate to a method for producing insoluble alpha-glucan of the present invention. Such a method includes, for example, the following steps: (a) providing an insoluble alpha-glucan produced in an enzymatic reaction comprising at least water, sucrose, and a glucosyltransferase enzyme for synthesizing insoluble alpha-glucan, wherein the insoluble alpha-glucan has at least about 200 DPw or DPn, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds; (b) hydrolyzing the insoluble alpha-glucan (precursor) to insoluble alpha-glucan particles having, for example, about 35 to about 100 (or, for example, up to about 200) DPw or DPn, carried out under aqueous conditions at a pH of 2.0 or less; and (c) optionally isolating the insoluble alpha-glucan particles produced in step (b). Step (b) of this method can optionally be characterized as an "acid hydrolysis" method or reaction.

[0071] Step (a) of the method for producing insoluble alpha-glucan particles according to this specification relates to providing an insoluble alpha-glucan precursor, which then proceeds to a hydrolysis step (b). The insoluble "alpha-glucan precursor" according to this specification is an insoluble alpha-glucan in itself, but has a molecular weight greater than that of an insoluble alpha-glucan produced by an acid hydrolysis method. Insoluble alpha-glucan precursors have glycosidic bond profiles as disclosed above (e.g., at least about 50%, 60%, 70%, 80%, 90%, 95%, 99%, or 100% alpha-1,3 glycosidic bonds) and, for example, about or at least about 200, 300, 400, 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400, 1500, 1600, 1650, 200-1650, 300-1650, It has DPw or DPn values ​​of 400-1650, 500-1650, 600-1650, 700-1650, 200-1250, 300-1250, 400-1250, 500-1250, 600-1250, 700-1250, 200-1000, 300-1000, 400-1000, 500-1000, 600-1000, 700-1000, 200-900, 300-900, 400-900, 500-900, 600-900, or 700-900.

[0072] The insoluble alpha-glucan precursors described herein are produced by an enzymatic reaction comprising at least water, sucrose, and a glucosyltransferase enzyme that synthesizes insoluble alpha-glucan. Glucosyltransferases, reaction conditions, and / or processes considered useful for producing the insoluble alpha-glucan precursors described herein are, for example, U.S. Patent Nos. 7,000,000, 8871474, 10301604, and 10260053, U.S. Patent Application Publication Nos. 2019 / 0112456 and 2019 / 0078062. Disclosed in the detailed specifications, Specification No. 2019 / 0078063, Specification No. 2018 / 0340199, Specification No. 2018 / 0021238, Specification No. 2018 / 0273731, Specification No. 2017 / 0002335 and Specification No. 2015 / 0064748, and International Publication No. 2017 / 079595 (all of which are incorporated herein by reference).

[0073] In some embodiments, glucosyltransferase enzymes for producing insoluble alpha-glucan precursors may contain amino acid sequences that are 100% identical or at least 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 98.5%, 99%, or 99.5% identical to amino acid residues 55-960 of SEQ ID NO: 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, 26, 28, 30, 34, or 59, or amino acid residues 55-960 of SEQ ID NO: 4, residues 54-957 of SEQ ID NO: 65, residues 55-960 of SEQ ID NO: 30, residues 55-960 of SEQ ID NO: 28, or residues 55-960 of SEQ ID NO: 20, and may have glucosyltransferase activity. These amino acid sequences are disclosed in U.S. Patent Application Publication No. 2019 / 0078063 (incorporated herein by reference). Furthermore, glucosyltransferase enzymes containing amino acid residues 55-960 of SEQ ID NOs: 2, 4, 8, 10, 14, 20, 26, 28, 30, 34 or SEQ ID NO: 4, residues 54-957 of SEQ ID NO: 65, residues 55-960 of SEQ ID NO: 30, residues 55-960 of SEQ ID NO: 28, or residues 55-960 of SEQ ID NO: 20 can synthesize insoluble alpha-glucan containing at least approximately 90% (approximately 100%) alpha-1,3 linkages. Any of the above glucosyltransferase enzyme amino acid sequences can be denatured as follows to increase the product yield.

[0074] In some embodiments, insoluble alpha-glucan can be synthesized from a glucosyltransferase enzyme for producing an insoluble alpha-glucan precursor in a yield of at least about 40%. In some embodiments, the yield of insoluble alpha-glucan by the glucosyltransferase enzyme may be about or at least about 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 91%, 92%, 93%, 94%, 95%, or 96%. In some embodiments, the yield may be evaluated based on the glucosyl component of the reaction. In some embodiments, the yield may be measured using HPLC or NIR spectroscopy. The yield can be achieved, for example, in a reaction carried out for about 16–24 hours (e.g., about 20 hours). An example of such a glucosyltransferase enzyme is one having an amino acid sequence that is modified to produce more products (insoluble alpha-glucan precursor and fructose) and fewer by-products (e.g., glucose, oligosaccharides such as leucose) from a given amount of sucrose substrate. For example, one, two, three, four or more amino acid residues in the catalytic domain of the glucosyltransferase of the present invention can be modified / substituted to obtain an enzyme that produces more products. Examples of suitable modified glucosyltransferase catalysts are disclosed in Tables 3-7 of U.S. Patent Publication No. 2019 / 0078063. A modified glucosyltransferase enzyme may include, for example, one or more amino acid substitutions corresponding to those in Tables 3-7 (ibid.), which are associated with at least a 40% insoluble alpha-glucan yield (as disclosed in U.S. Patent Publication No. 2019 / 0078063, the position numbering of such at least one substitution corresponds to the position numbering in Sequence ID No. 62). For example, a series of amino acid denaturations as shown in Table 6 or 7 (same as above) can be used.

[0075] In some embodiments, the alpha-glucan precursor may be a graft copolymer as disclosed in International Publication No. 2017 / 079595 or U.S. Patent Application Publication No. 2019 / 0185893 (these documents are incorporated herein by reference). Such a graft copolymer comprises dextran (as the main chain) and alpha-1,3-glucan (as the side chain). The latter component is grafted onto the former component, and typically, this graft copolymer is produced by using dextran or alpha-1,2-branched dextran as a primer for alpha-1,3-glucan synthesis by a glucosyltransferase that produces the alpha-1,3-glucan described above. In some embodiments, the graft copolymer comprises, for example, about or at least about 10% by weight, 20% by weight, 30% by weight, 35% by weight, 40% by weight, 45% by weight, 50% by weight, 55% by weight, 60% by weight, 65% by weight, 70% by weight, 35-65% by weight, 35-60% by weight, 35-55% by weight, 40-65% by weight, 40-60% by weight, 40-55% by weight, 45-65% by weight, 45-60% by weight, 45-55% by weight, 50-65% by weight, 50-60% by weight, or 50-55% by weight or less of a dextran main chain, with the remainder of the graft copolymer being alpha-1,3-glucan side chains. The alpha-1,3-glucan side chains of the alpha-glucan graft copolymers herein may be alpha-1,3-glucans disclosed herein. The dextran backbone of the alpha-glucan graft copolymers described herein shall contain approximately 100% alpha-1,6 glycosidic bonds (i.e., a fully linear dextran backbone) or approximately or at least approximately 90%, 95%, 96%, 97%, 98%, 99%, or 99.5% alpha-1,6 glycosidic bonds (i.e., a substantially linear dextran backbone). It is possible and / or for example, about or at least about 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 35, 40, 45, 50, 85, 90, 95, 100, 105, 110, 150, 200, 250, 300, 400, 500, 8~20,8-30, 8-100, 8-500, 3-4, 3-5, 3-6, 3-7, 3-8, 4-5, 4-6, 4-7, 4-8, 5-6, 5-7, 5-8, 6-7, 6-8, 7-8, 90-120, 95-120, 100-120, 105-120, 110-120, 115-120, 90-115, 95-115 It may have a DP or DPw of 100-115, 105-115, 110-115, 90-110, 95-110, 100-110, 105-110, 90-105, 95-105, 100-105, 90-100, 95-100, 90-95, 85-95, or 85-90 or less. In some embodiments, the dextran backbone (before being assembled into the graft copolymer) was alpha-1,2 branched, but the percentage of alpha-1,2 branching in the backbone of the graft copolymers herein may be, for example, about or at least about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 2-25%, 2-20%, 2-15%, 2-10%, 5-25%, 5-20%, 5-15%, 5-10%, 7-13%, 8-12%, 9-11%, 10-25%, 10-20%, or 10-15% or less. In some embodiments, the dextran backbone of the alpha-glucan graft copolymer is (A) (i) about 87-91.5% by weight glucose linked only at positions 1 and 6; (ii) about 0.1-1.2% by weight glucose linked only at positions 1 and 3; (iii) about 0.1-0.7% by weight glucose linked only at positions 1 and 4; (iv) about 7.7-8.6% by weight glucose linked only at positions 1, 3 and 6; and (v) (a) at positions 1, 2 and 6, or (b) 1 (B)(i) Approximately 0.4-1.7% by weight of glucose linked only at positions 1, 4 and 6; or (B)(i) Approximately 89.5-90.5% by weight of glucose linked only at positions 1 and 6; (ii) Approximately 0.4-0.9% by weight of glucose linked only at positions 1 and 3; (iii) Approximately 0.3-0.5% by weight of glucose linked only at positions 1 and 4; (iv) Approximately 8.0-8.3% by weight of glucose linked only at positions 1, 3 and 6; and (v)(a) Only at positions 1, 2 and 6, or (b) Only at position 1,It may contain approximately 0.7–1.4% by weight of glucose bonded only at positions 4 and 6. The molecular weight of such a dextran backbone (or any other dextran backbone specified herein) is, for example, approximately or at least approximately 100,000, 125,000, 150,000, 175,000, 200,000, 240,000, 250,000, 500,000, 750,000, 1,000,000, 2,000,000, 3,000,000, 4,000,000, 5,000,000, 6,000,000, 7,000,000, 8,000,000, 9,000,000, 10,000,000, 20,000,000, 30,000,000, 40,000,000, 50,000,000, 60,000,000, 70,000,000, 80,000,000, 90,000,000, 100,000,000, 110,000,000, 120,000,000, 130,000,000, 140,000,000, 150,000,000,000 60 million, 170 million, 180 million, 190 million, 200 million, 100,000-200,000, 125,000-175,000, 130,000-170,000, 135,000-165,000, 140,000-160,000, 145,000-155,000, 10 million-80 million, 20 million-70 million, 30 million-60 million, 40 million-50 million, 50 million-200 million, 60 million-200 million, 70 million-200 million, 80 million-200 million, 90 million-200 million, 100 million-200 million, 110 million-200 million, 120 million-200 million, 50 million-180 million, 60 million-180 million 10,000, 70 million to 180 million, 80 million to 180 million, 90 million to 180 million, 100 million to 180 million to 110 million to 180 million, 120 million to 180 million, 50 million to 160 million, 60 million to 160 million, 70 million to 160 million, 80 million to 160 million, 90 million to 160 million, 100 million to 160 million, 110 million to 160 million, 120 million to 160 million, 50 million to 140 million, 60 million to 140 million, 70 million to 140 million 10,000, 80 million to 140 million, 90 million to 140 million, 100 million to 140 million, 110 million to 140 million, 120 million to 140 million, 50 million to 120 million, 60 million to 120 million, 70 million to 120 million, 80 million to 120 million, 90 million to 120 million, 90 million to 110 million, 100 million to 120 million, 110 million to 120 million, 50 million to 110 million, 60 million to 110 million, 70 million to 110 million, 80 million to 110 millionThe Daltons may be 90 million to 110 million, 100 million to 110 million, 50 million to 100 million, 60 million to 100 million, 70 million to 100 million, 80 million to 100 million, 90 million to 100 million, or 95 million to 105 million. Before the graft copolymer of this specification enters hydrolysis step (b), the graft copolymer may be soluble, partially soluble, or insoluble. In some embodiments, before entering hydrolysis step (b), the graft copolymer is first treated with a dextranase (disclosed, for example, in U.S. Patent Application Publication No. 2017 / 0218093, incorporated herein by reference) to remove part or all of the dextran backbone of the copolymer (e.g., about or at least about 20%, 40%, 60%, 70%, 80%, 90%, 95%, or 99% by weight of the backbone). Optionally, this step may be performed after the hydrolysis step (b).

[0076] The temperature of the enzymatic reaction for producing the insoluble alpha-glucan precursor may be controlled as needed and may be, for example, about 5–50°C, 20–40°C, 30–40°C, 20–30°C, 20–25°C, 20°C, 25°C, 30°C, 35°C, or 40°C. The enzymatic reaction may be carried out for, for example, about 1, 1.5, 2, 2.5, 3, 3.5, 4, 6, 8, 10, 12, 14, 16, 18, 20, 22, 24, 36, 48, 60, 72, 96, 120, 144, 168, 1–4, 1–3.5, 1–3, 1.5–4, 1.5–3.5, 1.5–3, 2–4, 2–3.5, or 2–3 hours. In some aspects, the pH of the enzymatic reaction may be approximately 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 4.0–9.0, 4.0–8.5, 4.0–8.0, 5.0–8.0, 5.5–7.5, or 5.5–6.5.

[0077] The initial concentration of sucrose in the enzymatic reaction for producing an insoluble alpha-glucan precursor may be approximately or at least approximately 10, 15, 20, 25, 30, 40, 45, 50, 55, 60, 80, 90, 95, 100, 105, 110, 125, 150, 200, 300, 400, 500, 600, 10-50, 10-40, 10-30, 10-25, 15-50, 15-40, 15-30, or 15-25 g / L or less, or between any two of these values. "Initial concentration of sucrose" refers to the concentration of sucrose in the reaction composition immediately after all reaction components (e.g., at least water, sucrose, and glucosyltransferase enzyme) have been added / combined.

[0078] In some embodiments, the enzymatic reaction for producing an insoluble alpha-glucan precursor may further include a soluble gluco-oligosaccharide by-product from a previously performed enzymatic reaction that produced an insoluble alpha-glucan having at least 50% alpha-1,3-links. For example, to produce an insoluble alpha-glucan precursor, a soluble fraction (e.g., filtrate, precipitate) obtained from an enzymatic reaction that produced an insoluble alpha-glucan having at least 50% (e.g., ≥95% or 99%) alpha-1,3-links can be added to the enzymatic reaction herein. Such a soluble fraction contains a soluble gluco-oligosaccharide by-product. Various methods applicable to this method herein are disclosed in U.S. Patent Application Publication No. 2018 / 0340199 (incorporated herein by reference).

[0079] Prior to performing the hydrolysis step (b), the insoluble alpha-glucan precursor may be optionally isolated after its enzymatic preparation (as described above). In some embodiments, isolation of the insoluble alpha-glucan precursor may include performing at least the steps of centrifugation, filtration, fractionation, chromatographic separation, dialysis, evaporation, or dilution. Isolation of the insoluble alpha-glucan precursor may include at least the step of preparing a cake of the insoluble alpha-glucan precursor. Preparation of the cake may include, for example, performing at least the steps of centrifugation (the cake being pelletized alpha-glucan) and / or filtration (the cake being filtered alpha-glucan). Isolation may optionally further include washing the centrifuged and / or filtered insoluble alpha-glucan precursor once, twice, or more times with water or other aqueous liquids. The washing volume may optionally be at least about 10-100% of the volume of the reaction composition used to produce the alpha-glucan. Washing may be carried out in various ways, such as displacement washing or slurry washing, as needed. In some embodiments, the aqueous portion of the resulting cake may be free of (detectable) dissolved sugars or may contain about 0.1–1.5, 0.1–1.25, 0.1–1.0, 0.1–0.75, 0.1–0.5, 0.2–0.6, 0.3–0.5, 0.3–0.4, 0.2, 0.3, 0.4, 0.5, or 0.6% by weight or less of dissolved sugars. Such dissolved sugars may include, for example, sucrose, fructose, glucose, leucrose, and / or soluble gluco-oligosaccharides. The insoluble alpha-glucan precursor cake according to this specification may remain, for example, in a moist ("not dried") state and, in some embodiments, may contain (i) about 50%–90% by weight of water or aqueous solution, and (ii) about 10%–50% by weight of insoluble alpha-glucan precursor.In some embodiments, the cake may contain, for example, about 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 10-50, 10-40, 10-30, 10-20, 20-50, 20-40, 20-30, 30-50, 30-40, 40-50, 30-45, 35-45, 37.5-42.5, 35-40, or 40-45% by weight of insoluble alpha-glucan precursor (with up to 100% by weight of water or aqueous solution added). In some embodiments, the aqueous portion of the cake may have a solute and / or pH profile as described herein for aqueous solutions.

[0080] The isolation described herein may optionally further include drying the alpha-glucan precursor and / or preparing a dispersion of the alpha-glucan precursor. The isolated insoluble alpha-glucan precursor described herein, provided in dried / dried form, may contain, for example, about 12, 10, 8, 6, 5, 4, 3, 2, 1.5, 1.0, 0.5, 0.25, 0.10, 0.05 or 0.01% by weight or less of water. Drying can be carried out using an oven, freeze-drying, spray drying and / or by agitated air drying (e.g., rotary drying such as agitated filter / film drying, fluidized bed drying, or drum drying under vacuum). In some embodiments, drying can be at temperatures of, for example, about or at least about 20, 25, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 20-140, 20-130, 30-50, 35-45, 90-110, or 95-105°C. The dispersions described herein may contain about 0.1, 0.25, 0.4, 0.5, 0.75, 1.0, 1.25, 1.5, 1.75, 2.0, 2.25, 2.5, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0, 10, 0.5-10, 1-10, 2-10, 3-10, 4-10, or 5-10% by weight of an insoluble alpha-glucan precursor in water or an aqueous liquid, and may be, for example, a dispersion of either an undried or dried alpha-glucan precursor.

[0081] Step (b) of the method for producing insoluble alpha-glucan particles according to this specification relates to hydrolyzing the (above) insoluble alpha-glucan to insoluble alpha-glucan particles under aqueous conditions, typically at a pH of 2.0 or less. A dried or undried alpha-glucan precursor (above) can be added to the hydrolysis reaction. In some embodiments, the dispersion according to this specification is first prepared, and therefore the pH is subsequently lowered to initiate the hydrolysis of the insoluble alpha-glucan precursor to an insoluble alpha-glucan with a lower molecular weight.

[0082] The pH of the hydrolysis reaction described herein may be, for example, 2.0 or less. In some embodiments, the pH may be about 3.5, 3.0, 2.5, 2.0, 1.5, 1.0, 0.8, 0.6, 0.5, 0.4, 0.3, 0.2, 0.1, 0.05, 0.03, 0.01, 0.0, 0.0-2.0, 0.0-1.0, 0.0-0.5, 0.05-2.0, 0.05-1.0, 0.05-0.5, 0.1-2.0, 0.1-1.0 or 0.1-0.5 or less. Therefore, to achieve the low pH disclosed above, strong inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, hydroiodic acid or perchloric acid can be used. For example, an inorganic acid can be added to a dispersion of an insoluble alpha-glucan precursor until the desired pH is reached, thereby initiating the hydrolysis reaction. The hydrolysis reactions described herein are typically carried out under aqueous conditions, and the reaction liquid comprises a solvent which is water or an aqueous solution containing at least about 60, 70, 80, 90, 95, 98, or 99% by weight of water. However, in some other embodiments, the hydrolysis reactions described herein can be carried out by exposing a dry or wet insoluble alpha-glucan precursor to hydrogen chloride gas (for example, at a pressure of about or up to about 100 kPa).

[0083] The temperature of the hydrolysis reaction described herein may be, for example, about or at least about 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115, 120, 125, 130, 20-25, 20-30, 40-130, 40-125, 40-120, 70-130, 70-125, 70-120, 80-130, 80-125, 80-120, 60-100, 60-90, 70-100, 70-90, 75-100, 75-90 or 75-85°C or less.

[0084] The hydrolysis reactions described herein may proceed over, for example, about 1, 1.5, 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, 22, 24, 30, 36, 42, 48, 60, 72, 96, 120, 144, 168, 192, 1-192, 1-120, 1-72, 6-192, 6-120, 6-72, 8-192, 8-120, 8-72, 20-192, 20-120, or 20-72 hours. In some embodiments, the hydrolysis reaction described herein may proceed until the DPw of the hydrolyzed insoluble alpha-glucan is about 35–100 (e.g., 35–60, 40–60, 40–100), after which the DPw no longer decreases (e.g., does not fall below DPw 35 or 40). Typically, the hydrolysis reaction is carried out by stirring (e.g., stirring, shaking).

[0085] If necessary, the pH of the hydrolysis reaction can be neutralized (e.g., to pH 6-8), or it can be increased to a pH higher than 2, 3, 4, 5, or 6 after the reaction is complete. Neutralization can typically be achieved by adding a base such as a hydroxide (e.g., NaOH) or a bicarbonate (e.g., NaHCO3).

[0086] The insoluble alpha-glucan particle product of the reaction can be optionally isolated (e.g., washed, dispersed, and / or dried) by following any of the above procedures for the isolation / processing of the enzymatically synthesized insoluble alpha-glucan precursor (step c). In some embodiments, the isolated (optionally characterized as "purified") insoluble alpha-glucan particles may be present in the composition in at least about 50%, 60%, 70%, 80%, 85%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 98.5%, 99%, 99.5%, 99.8%, or 99.9% by weight (on a dry weight basis). Such isolated insoluble alpha-glucan particles can be used, for example, as an ingredient / component in the product / application.

[0087] The DPw or DPn of the insoluble alpha-glucan product of the hydrolysis reaction described herein may be, for example, about 35 to 100 (or, for example, up to about 100). In some embodiments, its DPw or DPn may be about 35 to 100, 35 to 90, 35 to 80, 35 to 70, 35 to 60, 35 to 55, 35 to 50, 40 to 100, 40 to 90, 40 to 80, 40 to 70, 40 to 60, 40 to 55, 40 to 50, 45 to 100, 45 to 90, 45 to 80, 45 to 70, 45 to 60, 45 to 55, or 45 to 50.

[0088] Any of the features disclosed herein with respect to insoluble alpha-glucan particles (e.g., glycosidic bond profile, crystallinity, plate characteristics and weight % content of plate, diameter, dispersion stability, dispersion viscosity, optical transparency, and pigment extender capacity) can similarly characterize the insoluble alpha-glucan products of the hydrolysis methods of this disclosure.

[0089] Some embodiments of this disclosure relate to methods for providing aqueous compositions containing insoluble alpha-glucan particles. Such methods typically include (a) providing the insoluble alpha-glucan particles disclosed herein, and (b) dispersing the particles in an aqueous liquid to produce an aqueous composition containing the insoluble alpha-glucan particles. Such methods may optionally be characterized as dispersion methods.

[0090] The insoluble alpha-glucan particles provided in step (a) of the dispersion method herein may be dry / dried or wet. The dry form of the alpha-glucan particles may contain, for example, about 12, 10, 8, 6, 5, 4, 3, 2, 1.5, 1.0, 0.5, 0.25, 0.10, 0.05 or 0.01% by weight or less of water. The wet form of the alpha-glucan particles may, in some embodiments, be a cake (filtered cake, wet cake). The cake of insoluble alpha-glucan particles herein may, for example, remain wet ("undried") and may, in some embodiments, contain (i) about 50% to 90% by weight of water or aqueous solution, and (ii) about 10% to 50% by weight of insoluble alpha-glucan particles. In some embodiments, the cake may contain, for example, about 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 10-50, 10-40, 10-30, 10-20, 20-50, 20-40, 20-30, 30-50, 30-40, 40-50, 30-45, 35-45, 37.5-42.5, 35-40, or 40-45% by weight of insoluble alpha-glucan particles (with up to 100% by weight of water or aqueous solution added). In some embodiments, the aqueous portion of the cake may have a solute and / or pH profile as described herein for aqueous solutions.

[0091] To carry out step (b) of dispersing the insoluble alpha-glucan particles, any suitable method may be utilized. In some embodiments, such dispersion can be carried out by applying high shear and / or other forms of mixing / stirring. High shear may be about or at least about 8, 9, 10, 11, or 12 kJ / kg in specific energy and / or may involve mixing at, for example, about or up to about 3000, 4000, 6000, 8000, 10000, 12000, 14000, or 15000 rpm. High shear and / or mixing / stirring may be applied for, for example, about 1, 2, 3, 4, 5, 6, 8, or 10 minutes or 2-4 minutes. Suitable means for shearing / mixing / agitating include, for example, dispersers, sonicators (e.g., ultrasonicators) (e.g., 40-60W, about 50W), homomixers, homogenizers (e.g., rotary or piston, rotor stator), microfluidicators, planetary mixers, colloid mills, jet mills, vortexes and / or any methodology described in International Publication No. 2016 / 030234, U.S. Patent Nos. 5,767,176, 6,139,875 and 8,722,092 and U.S. Patent Application Publication Nos. 2017 / 0055540 and 2018 / 0021238 (all of these documents are incorporated herein by reference). In some embodiments, high-shear mixing (such as that applied by any of the means described above) is not used to disperse insoluble alpha-glucan particles and achieve high viscosity; however, gentle mixing / vibration at low rpm / frequency (e.g., less than about 100, 50, or 30 rpm) is used in such embodiments to disperse insoluble alpha-glucan particles. The dispersions prepared herein may optionally be colloidal dispersions.

[0092] The aqueous compositions produced by the dispersion methods of this specification may contain, for example, about or at least about 0.1, 0.25, 0.4, 0.5, 0.75, 1.0, 1.25, 1.5, 1.75, 2.0, 2.25, 2.5, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0, 10.0, 0.5-10, 1-10, 2-10, 3-10, 4-10, or 5-10% by weight or less of insoluble alpha-glucan particles.

[0093] In some embodiments, the viscosity of the aqueous composition produced in step (b) of the dispersion method is at least about 10%, 50%, 75%, 100%, 500%, 1000%, 10000%, or 100000%, or 1000000%, (or any integer between 10% and 100000%) higher than the viscosity of the aqueous liquid present before step (b). Very large increases in viscosity can be obtained by the methods disclosed herein if the aqueous liquid before step (b) has little or no viscosity. The viscosity of aqueous compositions containing insoluble alpha-glucan particles as specified herein may be, for example, about or at least about 2.5, 5, 10, 100, 200, 300, 400, 500, 600, 700, 1000, 2000, 3000, 4000, 5000, 6000, 7000, 8000, 9000, 10000, or 15000 centipoise (cps). Viscosity may be measured using the aqueous composition at any temperature between about 3°C ​​and about 80°C (e.g., 4–30°C, 15–30°C, 15–25°C). Viscosity is typically measured at atmospheric pressure (about 760 Torre) or ±10% thereof. Viscosity can be measured, for example, using a viscometer or rheometer, and optionally, for example, about 0.1, 0.5, 1.0, 1.667, 2, 5, 10, 50, 100, 500, 1000, 0.1-500, 0.1-100, 1.0-500, 1.0-1000, or 1.0-100s. -1 Viscosity can be measured at a shear rate (rotational shear rate) of (1 / s). Optionally, viscosity can be measured according to the procedure outlined in the following examples.

[0094] It is noteworthy that the dispersions of insoluble alpha-glucan particles specified herein typically have enhanced viscosity (at any given shear rate) compared to insoluble alpha-glucans with a DPw > 200 (e.g., DPw ≥ about 700 or about 800), crystallinity < 0.65 (e.g., ≤ 0.60), and / or a D50 diameter of 5–50 microns (e.g., unhydrolyzed) (each polymer is provided in the same amount). Such viscosity enhancement may be about or at least about 10-fold, 25-fold, 50-fold, 75-fold, 100-fold, or 125-fold increase in viscosity (at any given shear rate). It is noteworthy that the dispersions of insoluble alpha-glucan particles specified herein typically maintain the same or similar (e.g., ±10%) viscosity profile / level, whether at a neutral pH (e.g., pH 6–8) or a low pH (e.g., pH ≤ 2 or 3) (the polymers are provided in the same amount).

[0095] The dried insoluble alpha-glucan particles (e.g., dried at least once following synthesis by hydrolysis) and the undried wet insoluble alpha-glucan particles (not dried following synthesis by hydrolysis) described herein can typically increase viscosity to the same or similar range as when dispersed under aqueous conditions (e.g., within about 10%, 20%, 30%, 40%, or 50% of the viscosity of the undried glucan dispersion), but it is worth noting that insoluble alpha-glucans (e.g., unhydrolyzed) with DPw > 200 (e.g., DPw ≥ about 700 or about 800), crystallinity < 0.65 (e.g., ≤ 0.60), and / or a D50 diameter of 5 to 50 microns do not typically exhibit this beneficial characteristic. When the latter alpha-glucan is dried at least once, it is typically not possible to increase its viscosity to the same or similar range as the undried wet form (for example, the viscosity of the dried glucan dispersion may be less than 10%, 5%, 2.5%, 1%, 0.5%, or 0.1% of the viscosity of the undried glucan dispersion).

[0096] It is noteworthy that the aqueous dispersions of insoluble alpha-glucan particles described herein typically possess enhanced stability in that the particles may remain dispersed after the dispersion is formed. For example, in the aqueous dispersions containing insoluble alpha-glucan particles described herein, the particles are dispersed through about or at least about 80%, 85%, 90%, 95%, 98%, 99%, or 100% of the volume of the dispersion. In some embodiments, such levels of dispersion are considered to be, optionally, at temperatures of approximately or up to approximately 15, 20, 25, 30, 35, 40, 50, 60, 70, or 80°C and / or at pH of approximately or up to approximately 0, 1, 2, 3, 4, 5, 6, 7, 8, or 9, over a period of time of at least approximately or up to approximately 0.5, 1, 2, 4, 6, 8, 10, 20, 30, 60, 90, 120, 150, 180, 210, 240, 270, 300, 330, or 360 hours or 1, 2, or 3 years (starting typically from the initial preparation of the dispersion) (any of these volume parameters and / or conditions may optionally be applied to the stable dispersions and stable emulsions defined above). In some embodiments, stability refers to particles having an enhanced ability to additionally or instead provide viscosity (e.g., any of the viscosity levels above, optionally for any of the above periods) to the aqueous composition and / or maintain the molecular weight (DPw) disclosed above. In some embodiments, a dispersion of insoluble alpha-glucan particles in an emulsion provides stability to the emulsion, and either the above-mentioned dispersion volume percentage and / or duration of such stability can similarly characterize the dispersed / emulsified droplets. In some embodiments, stability can additionally or alternatively characterize emulsions with relatively small droplet diameters (e.g., approximately 40, 38, 36, 34, 32, 30, 28, 26, 26-34, 26-32, 26-30, 28-34, 28-32 or 28-30 microns or less in diameter) and typically uniform in diameter (e.g., standard deviation of average diameter approximately 12, 11, 10, 9, 8, 7, 6, 5, 4, 5-10, 5-8, 6-10, 6-8 or less). A smaller average droplet diameter is equivalent to an increased total droplet surface area.In some embodiments, stability can additionally or alternatively characterize emulsions having an average storage modulus (Avg. G') (also called modulus) of about or at least about 40, 50, 60, 70, 80, 90, 100, 125, 150, 40-150, 40-125, 40-100, 50-150, 50-125, or 50-100 Pascals. The storage modulus of the emulsions herein can be measured according to the following examples or as disclosed, for example, in Varanasi et al. (2018, Frontiers Chem. 6:1-9, Article 409, incorporated herein by reference). Based on the above emulsion stabilizing effect of the insoluble alpha-glucan particles herein, it is conceivable that the particles could be used in applications / products where emulsion stabilization improves the performance of the application / product (although this is not a requirement for the particles used in the application / product). Examples of such applications / products can be disclosed herein, for example, dairy / dairy products (e.g., yogurt, ice cream, cream), mayonnaise, salad dressings, beverages / tonics (as carriers for supplying non-polar bioactive ingredients), cosmetic or pharmaceutical lotions / creams, water-based / latex paints, defoamers, rolling oils for metalwork, mining explosives, pesticide formulations, downhole fluids or pharmaceutical carriers or encapsulation systems for enhanced oil recovery operations, etc.

[0097] In some embodiments, emulsions containing insoluble alpha-glucan particles may further contain fibrils containing alpha-glucan with alpha-1,3 linkages. The alpha-glucan linkage and / or molecular weight profile of the fibrils herein are as disclosed herein with respect to insoluble alpha-glucan particles. Alpha-glucan fibrils may be as disclosed in U.S. Patent Application Publication 2018 / 0119357 (incorporated herein by reference). In some embodiments, the inclusion of fibrils in the emulsion may have a synergistic effect with the insoluble particles on emulsion stability. The concentration of fibrils in the emulsions herein may be any of the concentrations disclosed herein with respect to insoluble alpha-glucan particles in aqueous compositions.

[0098] In some embodiments, insoluble alpha-glucan particles dispersed in a liquid such as water or an aqueous solution have a light scattering effect on the liquid. For example, visible light can be scattered in arbitrary units (au) of about, at least about, or at most about 0.1, 0.25, 0.5, 0.75, 1.0, 1.25, 1.5, 1.75, 2.0, 2.25, 2.5, 2.75, or 3.0. In some embodiments, visible light can have wavelengths of about 380-750, 380-700, 380-650, 380-600, 380-550, 425-750, 425-700, 425-650, 425-600, 425-550, 450-550, or 475-525 nm. With respect to light scattering, the concentration of insoluble alpha-glucan particles dispersed in the liquid may be, for example, any of the concentrations disclosed herein, or about or at least about 0.05–10, 0.1–10, 1–10, 0.05–8, 0.1–8, or 1–8% by weight. In additional or other embodiments, the insoluble alpha-glucan particles dispersed in the liquid do not absorb or absorb very little (e.g., <1%, <0.1%) of the visible light emitted at the time of dispersion.

[0099] The insoluble alpha-glucan particles of the present disclosure can be present in a composition such as an aqueous composition (e.g., a dispersion such as a colloidal dispersion) or a dry composition, for example, at about or at least about 0.01, 0.05, 0.1, 0.2, 0.25, 0.3, 0.4, 0.5, 0.6, 0.7, 0.75, 0.8, 0.9, 1.0, 1.2, 1.25, 1.4, 1.5, 1.6, 1.75, 1.8, 2.0, 2.25, 2.5, 3.0, 3.5, 4.0, 4.5, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, 98 or 99 wt% or w / v% or less or in a range between any two of these values. The liquid component of the aqueous composition can be an aqueous fluid such as, for example, water or an aqueous solution. The solvent of the aqueous solution is typically water or can contain, for example, about or at least about 10, 20, 30, 40, 50, 60, 70, 80, 90, 95, 98 or 99 wt% of water.

[0100] In some embodiments, the aqueous solution of the aqueous composition has no (detectable) dissolved saccharides or has from about 0.1 to 1.5, 0.1 to 1.25, 0.1 to 1.0, 0.1 to 0.75, 0.1 to 0.5, 0.2 to 0.6, 0.3 to 0.5, 0.2, 0.3, 0.4, 0.5 or 0.6 wt% of dissolved saccharides. Such dissolved saccharides can include, for example, sucrose, fructose, leucrose and / or soluble gluco-oligosaccharides. In some embodiments, the aqueous solution of the aqueous composition has one or more salts / buffers (e.g., Na + , Cl -(NaCl, phosphate, tris, citrate) (e.g., ≤0.1, 0.5, 1.0, 2.0 or 3.0 by weight) and / or for example, about or about 0.0, 0.01, 0.03, 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.8, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6. The pH can be 0, 6.5, 7.0, 7.5, 8.0, 8.5, 0.0-1.0, 0.0-2.0, 0.0-3.0, 0.0-4.0, 0.0-5.0, 9.0, 4.0-9.0, 4.0-8.5, 4.0-8.0, 5.0-9.0, 5.0-8.5, 5.0-8.0, 6.0-9.0, 6.0-8.5, or less than 6.0-8.0. In some embodiments, the aqueous composition comprising the insoluble alpha-glucan particles herein may be an acid hydrolysis reaction as disclosed herein, and the aqueous portion of the reaction may correspondingly have a low pH (as described above).

[0101] Aqueous compositions (e.g., aqueous dispersions) containing insoluble alpha-glucan particles as specified herein may have viscosities of, for example, about or at least about 2.5, 5, 10, 100, 200, 300, 400, 500, 600, 700, 1000, 2000, 3000, 4000, 5000, 6000, 7000, 8000, 9000, 10000, or 15000 centipoise (cps). Viscosity can be measured as disclosed in the above or below examples. Typically, the insoluble alpha-glucan particles in the aqueous dispersion are dispersed through about or at least about 80%, 85%, 90%, 95%, 98%, 99%, or 100% of the volume of the dispersion.

[0102] The temperatures of compositions containing insoluble alpha-glucan particles as specified herein (e.g., aqueous compositions) are, for example, approximately or maximum of approximately 0, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115, 120, 125, 130, 5-5 The temperature can be 0, 20-25, 20-30, 20-40, 30-40, 40-130, 40-125, 40-120, 70-130, 70-125, 70-120, 80-130, 80-125, 80-120, 60-100, 60-90, 70-100, 70-90, 75-100, 75-90, or 75-85°C.

[0103] The compositions comprising insoluble alpha-glucan particles as described herein may be non-aqueous (e.g., dry compositions) in some embodiments. Examples of such embodiments include powders, granules, microcapsules, flakes, or any other form of particulate matter. Other examples include larger compositions such as pellets, bars, kernels, beads, tablets, sticks, or other aggregates. Non-aqueous or dry compositions typically contain about 12, 10, 8, 6, 5, 4, 3, 2, 1.5, 1.0, 0.5, 0.25, 0.10, 0.05, or 0.01% by weight or less of water. In some embodiments (e.g., relating to laundry or dishwashing detergents), the dry compositions as described herein may be provided in sachets or pouches.

[0104] The compositions comprising insoluble alpha-glucan particles herein may, in some embodiments, contain one or more salts such as sodium salts (e.g., NaCl, Na2SO4). Other non-limiting examples of salts include (i) aluminum, ammonium, barium, calcium, chromium (II or III), copper (I or II), iron (II or III), hydrogen, lead (II), lithium, magnesium, manganese (II or III), mercury (I or II), potassium, silver, sodium, strontium, tin (II or IV), or zinc cations, and (ii) acetates, borates, bromates, bromides, carbonates, chlorates, chlorides, chlorites, chromates, cyanamides, Examples include those having cyanide, dichromate, dihydrogen phosphate, ferricyanide, ferrocyanide, fluoride, bicarbonate, hydrogen phosphate, hydrogen sulfate, hydrogen sulfide, bisulfite, hydride, hydroxide, hypochlorite, iodate, iodide, nitrate, nitride, nitrite, oxalate, oxide, perchlorate, permanganate, peroxide, phosphate, phosphite, phosphate, silicate, stannate, stannate, sulfate, sulfide, sulfite, tartrate, or thiocyanate anions. Therefore, for example, any salt having a cation from (i) above and an anion from (ii) above may be included in the composition. Salts may be present in the aqueous compositions herein in weight percent of, for example, about or at least about 0.01, 0.025, 0.05, 0.075, 0.1, 0.25, 0.5, 0.75, 1.0, 1.25, 1.5, 1.75, 2.0, 2.5, 3.0, 3.5, 0.01-3.5, 0.5-3.5, 0.5-2.5, or 0.5-1.5% by weight (such weight percent values ​​typically refer to the total concentration of one or more salts).

[0105] The compositions comprising insoluble alpha-glucan particles described herein may optionally contain one or more active enzymes. Examples of suitable enzymes include proteases, cellulases, hemicellulases, peroxidases, lipolytic enzymes (e.g., metallolipolytic enzymes), xylanases, lipases, phospholipases, esterases (e.g., arylesterases, polyesterases), perhydrolases, cutinases, pectinases, pectinate lyases, mannanases, keratinases, reductases, oxidases (e.g., choline oxidases), phenol oxidases, lipoxygenases, ligninases, pullulanases, tanases, pentosanases, melanases, beta-glucanases, arabinosidases, hyaluronidases, chondroitinases, laccases, metalloproteinases, amadriases, glucoamylases, arabinofuranosidases, phytases, isomerases, transferases, nucleases, and amylases. Where enzymes are present, they may be included in the compositions herein in the form of active enzymes at a concentration of approximately 0.0001 to 0.1% by weight (e.g., 0.01 to 0.03% by weight), for example (calculated as pure enzyme protein). For textile care applications, enzymes (e.g., any of the above, such as cellulase) may be present in the aqueous composition (e.g., washing solution) in which the textile is treated at a concentration of total enzyme protein ranging from a minimum of approximately 0.01 to 0.1 ppm or a total enzyme protein of approximately 0.1 to 10 ppb (e.g., less than 1 ppm) to a maximum of approximately 100, 200, 500, 1,000, 2,000, 3,000, 4,000, or 5,000 ppm in the aqueous composition (e.g., washing solution) in which the textile is treated.

[0106] The compositions comprising the insoluble alpha-glucan particles herein, for example, aqueous or non-aqueous compositions (as described above), may be in the form of, for example, household care products, personal care products, industrial products, ingestible products (e.g., food) or pharmaceutical products. Examples of such products are U.S. Patent Publication Nos. 2018 / 0022834, 2018 / 0237816, 2018 / 0230241, 20180079832, 2016 / 0311935, 2016 / 0304629, 2015 / 0232785, and 2015 / 0368594. This may be as described in any of the following publications: Specification No. 2015 / 0368595, Specification No. 2016 / 0122445, Specification No. 2019 / 0309096, or Specification No. 2019 / 0202942, or International Publication No. 2016 / 133734 and International Publication No. 2017 / 218391 (these are incorporated herein by reference). In some embodiments, compositions comprising insoluble alpha-glucan particles may comprise at least one component / ingredient of a household care product, personal care product, industrial product, pharmaceutical product, or ingestible product (e.g., food) as disclosed in any of the aforementioned publications and / or disclosed herein.

[0107] The insoluble alpha-glucan particles disclosed herein are considered useful for imparting one or more of the following physical properties to personal care products, pharmaceutical products, household products, industrial products, or ingestible products (e.g., food): for example, thickening, freeze-thaw stability, lubricity, moisture retention and release, texture, consistency, shape retention, emulsifying properties, binding properties, suspendability, dispersibility, gelling properties, and reduction of mineral hardness. Examples of concentrations or amounts of insoluble alpha-glucan particles in a product may be, for example, any of the weight percent provided herein.

[0108] Personal care products as disclosed herein include, but are not limited to, skincare compositions, cosmetic compositions, antifungal compositions, and antimicrobial compositions. Personal care products as disclosed herein may take the form of, for example, lotions, creams, pastes, mineral oils, ointments, pomades, gels, liquids, or combinations thereof. Personal care products disclosed herein may optionally contain at least one active ingredient. An active ingredient is generally recognized as an ingredient that produces an intended cosmetic or pharmacological effect.

[0109] In certain embodiments, skincare products can be applied to the skin to address skin damage associated with dehydration. Skincare products may also be used to address the appearance of the skin (e.g., to reduce the appearance of scaly, cracked, and / or reddened skin) and / or to address the texture of the skin (e.g., to reduce roughness and / or dryness of the skin while improving the smoothness and delicacy of the skin). Skincare products typically contain at least one active ingredient, such as zinc oxide, petrolatum, white petrolatum, mineral oil, cod liver oil, lanolin, dimethicone, hard fat, vitamin A, allantoin, calamine, kaolin, glycerin, or colloidal oatmeal, or combinations thereof, to treat or prevent skin diseases or to provide moisturizing effects to the skin while providing cosmetic effects. Skincare products may contain one or more natural moisturizing elements, such as ceramides, hyaluronic acid, glycerin, squalane, amino acids, cholesterol, fatty acids, triglycerides, phospholipids, glycosphingolipids, urea, linoleic acid, glycosaminoglycans, mucopolysaccharides, sodium lactate, or sodium pyrrolidone carboxylate. Other ingredients that may be included in skincare products include, but are not limited to, glycerides, apricot kernel oil, canola oil, squalane, squalene, coconut oil, corn oil, jojoba oil, jojoba wax, lecithin, olive oil, safflower oil, sesame oil, shea butter, soybean oil, sweet peach oil, sunflower oil, tea tree oil, shea butter, palm oil, cholesterol, cholesterol esters, wax esters, fatty acids, aloe vera, and orange oil.

[0110] Personal care products as defined herein may also be in the form of, for example, makeup, lipstick, mascara, lipstick, foundation, blush, eyeliner, lip liner, lip gloss, other cosmetics, sunscreen, sunblock, nail polish, nail conditioner, bath gel, shower gel, body soap, facial cleanser, lip balm, skin conditioner, cold cream, moisturizer, body spray, soap, body scrub, desquamant, astringent, scratching lotion, depilatory, permanent solution, anti-dandruff preparation, antiperspirant composition, deodorant, shaving products, pre-shave products, after-shave products, cleansing agents, skin gel, rinse, toothpaste composition, toothpaste, or mouthwash. Examples of personal care products (e.g., cleansers, soaps, scrubs, cosmetics) include carriers or scrubbing agents (e.g., jojoba beads [jojoba ester beads]) (e.g., about 1-10, 3-7, 4-6, or 5% by weight), and such active ingredients may be optionally dispersed within the product.

[0111] In some embodiments, personal care products may be hair care products. Examples of hair care products as used herein include shampoos, hair conditioners (leave-in or rinse-out), cream rinses, hair dyes, hair color products, hair shine products, hair serums, anti-frizzy products, split-end repair products, mousses, hair sprays, and styling gels. In some embodiments, hair care products may be in the form of liquids, pastes, gels, solids, or powders. The hair care products disclosed herein typically include one or more of the following ingredients commonly used in the formulation of hair care products: anionic surfactants, e.g., sodium polyoxyethylene lauryl ether sulfate; cationic surfactants, e.g., stearyltrimethylammonium chloride and / or distearyltrimethylammonium chloride; nonionic surfactants, e.g., glyceryl monostearate, sorbitan monopalmitate and / or polyoxyethylene cetyl ether; humectants, e.g., propylene glycol, 1,3-butylene glycol, glycerin, sorbitol, pyroglutamate, amino acids and / or trimethylglycine; hydrocarbons, e.g., liquid paraffin, petrolatum, solid paraffin, squalane and / or olefin oligomers; higher alcohols, e.g., stearyl alcohol and / or cetyl alcohol; superfatting agents; anti-dandruff agents; disinfectants; anti-inflammatory agents; herbal medicines; water-soluble polymers, e.g., methylcellulose, hydroxycellulose and / or partially deacetylated chitin; preservatives, e.g., parabens; UV absorbers; pearlescent agents; pH adjusters; fragrances; and pigments.

[0112] The pharmaceutical products described herein may be in the form of, for example, emulsions, liquids, elixirs, gels, suspensions, solutions, creams, or ointments. The pharmaceutical products described herein may also be in the form of any of the personal care products disclosed herein, such as antimicrobial or antifungal compositions. The pharmaceutical products may further comprise one or more pharmaceutically acceptable carriers, diluents, and / or pharmaceutically acceptable salts. The insoluble alpha-glucan particles disclosed herein may also be used in capsules, beads, pastels, capsule materials, tablets, tablet coatings, and as excipients for pharmaceuticals and medicines.

[0113] For example, the compositions herein containing insoluble alpha-glucan particles may be capsule materials. Capsule materials may be used, for example, to control and / or protect the release of materials and / or activators and / or compounds held within the capsule material. Capsule materials herein may encapsulate flavorings (e.g., any of those disclosed in U.S. Patent No. 7,196049, incorporated herein by reference), ingestible products (e.g., foods, beverages, flavorings, such as those disclosed in U.S. Patent No. 7,022352, incorporated herein by reference), pharmaceutical or health products (e.g., liquid drugs, prebiotics, probiotics), personal care products (e.g., toothpaste, mouthwash, face / body creams), and household care products (e.g., dry or liquid detergents, bleaches). For example, any suitable composition / product disclosed in other parts of this Spec. or in U.S. Patent Application Publication No. 2009 / 0209661 or No. 2007 / 0148105 (which are incorporated herein by reference, respectively, for example, in consumer products) may be encapsulated (with or without alpha-glucan particles). In some embodiments, the capsule materials herein may encapsulate hydrophobic or nonpolar compositions, for example, which may include lipids (e.g., oils, essential oils, fats, waxes, free fatty acids, glycerols, phospholipids, sterols, triglycerides, diglycerides, monoglycerides), alkanes, alkenes / olefins, hydrophobic aromatic or cyclic compounds, hydrophobic fragrance compounds and / or hydrophobic fragrances or nutrients. In some embodiments, the encapsulated products herein may be in a dry form. In some cases, the capsule materials may have the same or similar composition / formulation and / or thickness as the films or coatings herein that are suitable for use as capsule materials. The capsule material may contain, for example, about or at least about 50, 60, 70, 80, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, or 100% by weight of insoluble alpha-glucan particles.The capsule materials herein and / or other capsule materials may, in some embodiments, further comprise polyurethane, polyacrylate, polylactic acid, polysaccharides (in addition to alpha-glucan particles), gelatin, melamine, and / or formaldehyde. One or more additional additives that modify the mechanical, thermal, and / or decomposition profile of the capsule materials herein may be optionally included.

[0114] In some embodiments, the encapsulation compositions disclosed above can be produced by a method comprising (a) providing a liquid emulsion comprising at least the insoluble alpha-1,3-glucan herein, water, and a liquid / compound miscible in water (e.g., any hydrophobic or nonpolar substance disclosed herein), and (b) removing all or most (≥88%, 90%, 95%, 98%, 99%, 99.5%, 99.9% by weight) of water from the emulsion. Such removal may include drying by, for example, freeze-drying or spray-drying. The liquid emulsion may be provided by an encapsulation method (e.g., by mixing and / or homogenizing the emulsion components). In some embodiments, the temperature of the mixture to be emulsified is increased to aid emulsification. To liquefy / dissolve non-aqueous components (immiscible components), such as components that are solid at room temperature and thereby provide an immiscible liquid / compound in water, the temperature can be increased (e.g., to an increase of at least 1 or 2°C above the melting point of the immiscible component). The temperature increase of the emulsification is typically maintained until the emulsification enters the drying step. In the encapsulation method herein, it should be understood that with respect to the product of the method, an immiscible liquid / compound in water (or possibly a solid depending on its melting point) is encapsulated by a composition containing insoluble alpha-1,3-glucan. The conditions for preparing the encapsulated product herein by freeze-drying or spray-drying, etc. (e.g., temperature, pressure, time and / or airflow velocity) may be the same as or similar to the values ​​disclosed in Example 7 below (e.g., within 5%, 10%, 15%, or 20% of the specified values). In some other embodiments of the encapsulation method of this disclosure, alpha-1,3-glucan may be in the form of the alpha-glucan precursor herein.

[0115] The household and / or industrial products of this specification may be, for example, drywall tape bonding compounds; mortar; grout; cement plaster; spray plaster; cement stucco; adhesives; pastes; wall / ceiling binders; binders and processing aids for tape casting, extrusion molding, injection molding and ceramics; spray adhesives and suspension / dispersion aids for insecticides, herbicides and fertilizers; textile care products, for example, fabric softeners and laundry detergents; hard surface cleaners; air purifiers; polymer emulsions; latex; gels, for example, aqueous gels; surfactant solutions; paints, for example, aqueous paints; protective coatings; adhesives; sealants and caulking agents; inks, for example, aqueous inks; metal cutting fluids; films or coatings; or emulsion-based metal cleaning solutions used in electroplating, phosphate treatment, galvanizing and / or general metal cleaning operations.

[0116] Examples of edible products as described herein include foods, beverages, animal feed, animal health and / or nutrition products, and / or pharmaceuticals. The intended use of the insoluble alpha-glucan particles disclosed herein in edible products can provide chewiness, add volume, and / or thickness.

[0117] Further uses of the insoluble alpha-glucan particles of this disclosure for edible products include: puffing, binding and / or coating components; carriers for colorants, flavors / flavors and / or high-intensity sweeteners; spray-drying additives; leavening agents, thickeners, dispersants and / or emulsifiers; and components that promote moisture retention (humectants). Examples of prepareable products having the insoluble alpha-glucan particles of this specification include foods, beverages, pharmaceuticals, nutritional products and sports products. Examples of beverages of this specification include concentrated beverage mixtures, carbonated beverages, non-carbonated beverages, fruit-flavored beverages, fruit juices, tea, coffee, milk, nectar, powdered beverages, liquid concentrates, dairy beverages, ready-to-drink (RTD) products, smoothies, alcoholic beverages, flavored waters and combinations thereof. Examples of foods as used herein include baked goods (e.g., bread), confectionery, frozen dairy products, meat, artificial / synthetic / cultured meat, cereal products (e.g., breakfast cereals), dairy products (e.g., yogurt), spices (e.g., mustard, ketchup, mayonnaise), snack bars, soups, dressings, mixes, processed foods, baby food, diet foods, peanut butter, syrups, sweeteners, food coatings, pet food, animal feed, animal health and nutrition products, dried fruits, sauces, gravy, jams / jelly, dessert products, spreads, butter, breadcrumbs, spice mixes, sugar coatings, and the like. In some embodiments, insoluble alpha-glucan particles can provide or enhance the fizz of beverages (e.g., dairy beverages, non-dairy alternative beverages (e.g., "vegan" milks such as soy milk, almond milk, or coconut milk), dairy creamers and / or non-dairy creamers for hot beverages (e.g., coffee [e.g., cappuccino], tea [e.g., chai tea]).

[0118] The insoluble alpha-glucan particles disclosed herein may be included in, for example, personal care products, pharmaceutical products, household products, industrial products, or ingestible products (e.g., food) in amounts that provide the desired viscosity and / or dispersion. Examples of concentrations or amounts of insoluble alpha-glucan particles in a product are any of the weight percent provided above.

[0119] The compositions disclosed herein may be in the form of detergent compositions, such as textile care compositions. The textile care compositions herein can be used for hand washing, machine washing and / or other purposes, such as soaking and / or pre-treatment of textiles. The textile care compositions may be in the form of, for example, laundry detergents; textile conditioners, any laundry products, rinse products or dryer additives; unit doses or sprays. Liquid textile care compositions may be in the form of aqueous compositions disclosed herein. In other embodiments, the textile care compositions may be in dry form, such as granular detergents or dryer additive textile softener sheets. Other non-limiting examples of the textile care compositions herein include granular or powdered all-purpose or strong detergents; liquid, gel or paste all-purpose or strong detergents; liquid or dry detergents for fine (e.g., delicate) fibers; cleaning aids such as bleaching additives, "stain sticks" or pre-treatment agents; substrate loading products, such as dry or wet wipes, pads or sponges; sprays and mists.

[0120] The detergent compositions described herein may be in any useful form, such as powder, granules, paste, bar, unit dose, or liquid. Liquid detergents may typically be aqueous, containing up to about 70% by weight of water and 0% to about 30% by weight of an organic solvent. Liquid detergents may also be in the form of a compact gel containing only about 30% by weight of water.

[0121] The detergent compositions described herein typically comprise one or more surfactants, selected from nonionic surfactants, anionic surfactants, cationic surfactants, amphoteric surfactants, zwitterionic surfactants, semipolar nonionic surfactants, and mixtures thereof. In some embodiments, the surfactant is included in a concentration of about 0.1% to about 60% by weight of the detergent composition; in other embodiments, the concentration is about 1% to about 50% by weight; and in yet another embodiment, the concentration is about 5% to about 40% by weight. The detergent will typically contain 0% to about 50% by weight of anionic surfactants, such as linear alkylbenzene sulfonates (LAS), alpha-olefin sulfonates (AOS), alkyl sulfates (higher alcohol sulfates) (AS), alcohol ethoxysulfates (AEOS or AES), secondary alkanesulfonates (SAS), alpha-sulfo fatty acid methyl esters, alkyl- or alkenyl succinic acids, or soaps. Furthermore, the detergent composition may optionally contain 0% to about 40% by weight of nonionic surfactants, such as (for example, as described in International Publication No. 92 / 06154 incorporated herein by reference) alcohol ethoxylates (AEO or AE), carboxylated alcohol ethoxylates, nonylphenol ethoxylates, alkyl polyglycosides, alkyldimethylamine oxides, ethoxylated fatty acid monoethanolamines, fatty acid monoethanolamides, or polyhydroxyalkyl fatty acid amides.

[0122] The detergent compositions herein typically comprise one or more detergent builders or builder systems. In some embodiments, alpha-1,3-glucan oxide may be included as a cobuilder used with one or more further builders, such as any of those disclosed herein. Alpha-1,3-glucan oxide compounds for use herein are disclosed in U.S. Patent Application Publication No. 2015 / 0259439. In some embodiments incorporating at least one builder, the cleaning composition comprises the builder in an amount of at least about 1% by weight, about 3% to about 60% by weight, or further about 5% to about 40% by weight of the composition. Examples of builders (in addition to alpha-1,3-glucan oxide) include alkali metals, ammonium salts and alkanol-ammonium salts of polyphosphates, alkali metal silicates, alkaline earth and alkali metal carbonates, aluminosilicates, polycarboxylate compounds, ether hydroxypolycarboxylates, copolymers of maleic anhydride and ethylene or vinyl methyl ether, 1,3,5-trihydroxybenzene-2,4,6-trisulfonic acid and carboxymethyloxysuccinic acid, various alkali metal, ammonium and substituted ammonium salts of polyacetic acid, such as ethylenediaminetetraacetic acid and nitrilotriacetic acid, as well as polycarboxylates, such as meritic acid, succinic acid, citric acid, oxydisuccinic acid, polymaleic acid, benzene-1,3,5-tricarboxylic acid, carboxymethyloxysuccinic acid and their soluble salts, but are not limited to these. In fact, it is expected that the use of any suitable builder will be seen in various embodiments of this disclosure. Further examples of detergent builders or complexing agents include zeolites, diphosphates, triphosphates, phosphonates, citrates, nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DTMPA), alkylsuccinic acids and alkenylsuccinic acids, soluble silicates or layered silicates (e.g., SKS-6 from Hoechst).

[0123] In some embodiments, the builder forms water-soluble hard ion complexes (e.g., metal ion sequestering builders) such as citrates and polyphosphates (e.g., sodium tripolyphosphate, sodium tripolyphosphate hexahydrate, potassium tripolyphosphate, and mixed sodium tripolyphosphate-potassium). Any suitable builder, including builders known in the art, is expected to be used in this disclosure (see, for example, European Patent No. 2100949).

[0124] In some embodiments, suitable builders include phosphate builders and non-phosphate builders. In some embodiments, the builder is a phosphate builder. In some embodiments, the builder is a non-phosphate builder. The builder may be used in concentrations of 0.1% to 80% by weight, 5% to 60% by weight, or 10% to 50% by weight of the composition. In some embodiments, the product comprises a mixture of phosphate builders and non-phosphate builders. Suitable phosphate builders include monophosphates, diphosphates, triphosphates, or oligomeric polyphosphates, for example, alkali metal salts of these compounds, such as sodium salts. In some embodiments, the builder may be sodium tripolyphosphate (STPP). Furthermore, the composition may contain carbonates and / or citrates, preferably citrates, which help to achieve a neutral pH composition. Other suitable non-phosphate builders include homopolymers and copolymers of polycarboxylic acids and their partial or fully neutralized salts, monomeric polycarboxylic acids and hydroxycarboxylic acids, and their salts. In some embodiments, the salts of the above compounds include ammonium salts and / or alkali metal salts, i.e., lithium salts, sodium salts and potassium salts, for example, sodium salts. Suitable polycarboxylic acids include acyclic, alicyclic, heterocyclic and aromatic carboxylic acids, which in some embodiments may contain at least two carboxyl groups that can be separated from each other by two or fewer carbon atoms in some cases.

[0125] The detergent compositions herein may contain at least one chelating agent. Suitable chelating agents include, but are not limited to, copper, iron and / or manganese chelating agents and mixtures thereof. In embodiments using at least one chelating agent, the composition contains about 0.1% to about 15% by weight or further about 3.0% to about 10% by weight of the chelating agent of the composition.

[0126] The detergent compositions herein may contain at least one deposition aid. Suitable deposition aids include, but are not limited to, polyethylene glycol, polypropylene glycol, polycarboxylates, antifouling polymers such as polyterephthalic acid, clays such as kaolinite, montmorillonite, attapulgite, illite, bentonite, halloysite, and mixtures thereof.

[0127] The detergent compositions of this specification may contain one or more dye transfer inhibitors. Suitable polymer dye transfer inhibitors include, but are not limited to, polyvinylpyrrolidone polymers, polyamine N-oxide polymers, copolymers of N-vinylpyrrolidone and N-vinylimidazole, copolymers of polyvinyloxazolidone and polyvinylimidazole, or mixtures thereof. Further dye transfer inhibitors include manganese phthalocyanine, peroxidase, polyvinylpyrrolidone polymers, polyamine N-oxide polymers, N-vinylpyrrolidone and N-vinylimidazole, copolymers of polyvinyloxazolidone and polyvinylimidazole, and / or mixtures thereof. Examples of chelating agents include ethylenediaminetetraacetic acid (EDTA); diethylenetriaminepentamethylenephosphonic acid (DTPMP); hydroxyethane diphosphate (HEDP); ethylenediamine N,N'-disuccinate (EDDS); methylglycine diacetic acid (MGDA); diethylenetriaminepentaacetic acid (DTPA); propylenediaminetetraacetic acid (PDTA); 2-hydroxypyridine-N-oxide (HPNO); or methylglycine diacetic acid (MGDA); glutamic acid N,N-diacetic acid (N,N-diccarboxymethyl Examples include tetrasodium tyl glutamate (GLDA); nitrilotriacetic acid (NTA); 4,5-dihydroxy-m-benzenedisulfonic acid; citric acid and any salts thereof; N-hydroxyethylethylenediaminetriacetic acid (HEDTA), triethylenetetraaminehexaacetic acid (TTHA), N-hydroxyethyliminodiacetic acid (HEIDA), dihydroxyethylglycine (DHEG), ethylenediaminetetrapropionic acid (EDTP), and derivatives thereof that can be used alone or in combination with any of the above. In embodiments using at least one dye transfer inhibitor, the compositions herein may contain about 0.0001% to about 10% by weight, about 0.01% to about 5% by weight, or further about 0.1% to about 3% by weight of the composition.

[0128] The detergent compositions herein may contain silicates. In some of these embodiments, sodium silicates (e.g., sodium disilicate, sodium metasilicate, and / or crystalline phyllosilicate) are used. In some embodiments, the silicate is present in a concentration of about 1% to about 20% by weight of the composition. In some embodiments, the silicate is present in a concentration of about 5% to about 15% by weight of the composition.

[0129] The detergent compositions of this specification may contain dispersants. Suitable water-soluble organic materials include, but are not limited to, homopolymeric acids or copolymeric acids or salts thereof, in which the polycarboxylic acid contains at least two carboxyl groups separated from each other by two or fewer carbon atoms.

[0130] The detergent compositions herein may, for example, additionally contain one or more of the enzymes disclosed above. In some embodiments, the detergent composition may contain one or more enzymes and residual cleaning aids, each at a concentration of about 0.00001% to about 10% by weight of the composition. In some other embodiments, the detergent composition may also contain each enzyme at concentrations of about 0.0001% to about 10% by weight, about 0.001% to about 5% by weight, about 0.001% to about 2% by weight, or about 0.005% to about 0.5% by weight of the composition. The enzymes contained in the detergent compositions herein may be stabilized using conventional stabilizers, such as polyols such as propylene glycol or glycerol; sugars or sugar alcohols; lactic acid; boric acid or boric acid derivatives (e.g., aromatic boric acid esters).

[0131] In some embodiments, detergent compositions may contain one or more other types of polymers in addition to the insoluble alpha-glucan particles disclosed herein. Examples of other types of polymers useful herein include carboxymethylcellulose (CMC), dextran, poly(vinylpyrrolidone) (PVP), polyethylene glycol (PEG), poly(vinyl alcohol) (PVA), polycarboxylates, such as polyacrylates, maleic acid / acrylic acid copolymers, and lauryl methacrylate / acrylic acid copolymers.

[0132] The detergent compositions herein may contain a bleaching system. For example, the bleaching system may include a perborate or percarbonate that can be bound to an H2O2-derived peracid-forming bleaching activator, such as tetraacetylethylenediamine (TAED) or nonanoyloxybenzenesulfonate (NOBS). Alternatively, the bleaching system may include a peroxy acid (e.g., an amide, imide, or sulfone type peroxy acid). Alternatively, the bleaching system may further include an enzymatic bleaching system containing a perhydrolase, such as the system described in International Publication No. 2005 / 056783.

[0133] The detergent compositions described herein may also contain conventional detergent components such as fabric conditioners, viscosity enhancers, foaming agents, antifoaming agents, corrosion inhibitors, stain suspenders, anti-redeposition agents, dyes, disinfectants, anti-discoloration agents, fluorescent whitening agents, or fragrances. The pH of the detergent compositions described herein (measured in aqueous solution at the concentration used) is typically neutral or alkaline (for example, a pH of about 7.0 to about 11.0).

[0134] The insoluble alpha-glucan particles described herein may, if necessary, be included as anti-redeposition agents and / or clay stain removers in detergent compositions, such as textile care compositions (such active ingredients may optionally be characterized as whiteness maintainers in a given aspect). Examples of other suitable anti-redeposition agents and / or clay stain removers described herein include polyethoxyamphoteric surfactants, water-soluble copolymers of acrylic acid or methacrylic acid with acrylic acid or methacrylic acid-ethylene oxide condensate (e.g., U.S. Patent No. 3,719,647), cellulose derivatives, such as carboxymethylcellulose and hydroxypropylcellulose (e.g., U.S. Patents No. 3,597,416 and 3,523,088), and mixtures containing nonionic alkyl polyethoxy surfactants, polyethoxyalkyl quaternary cationic surfactants and fatty acid amide surfactants (e.g., U.S. Patent No. 4,228,044). Other suitable anti-redeposition and clay-based stain removers, non-limiting examples, are disclosed in U.S. Patent No. 4,597,898 and 4,891,160 and International Publication No. 95 / 32272 (all of which are incorporated herein by reference).

[0135] Specific forms of detergent compositions that can be adapted to the purposes disclosed herein include, for example, U.S. Patent Application Publication No. 20090209445A1, No. 20100081598A1, No. 7001878B2, European Patent No. 1504994B1, International Publication Brochure No. 2001085888A2, International Publication Brochure No. 2003089562A1, and International Publication Brochure No. 200909 Pamphlets No. 8659A1, No. 2009098660A1, No. 2009112992A1, No. 2009124160A1, No. 2009152031A1, No. 2010059483A1, No. 2010088112A1, No. 2010090915A1, and No. 20101352 Pamphlet No. 38A1, Pamphlet No. 2011094687A1, Pamphlet No. 2011094690A1, Pamphlet No. 2011127102A1, Pamphlet No. 2011163428A1, Pamphlet No. 2008000567A1, Pamphlet No. 2006045391A1, Pamphlet No. 2006007911A1, Pamphlet No. 201202740 This is disclosed in Brochure 4A1, European Patent No. 1740690B1, International Publication No. 2012059336A1, U.S. Patent No. 6730646B1, International Publication No. 2008087426A1, International Publication No. 2010116139A1, and International Publication No. 2012104613A1 (all of which are incorporated herein by reference).

[0136] The laundry detergent compositions described herein may optionally be strong (all-purpose) laundry detergent compositions. A typical strong laundry detergent composition contains a detergent surfactant (10% by weight to 40% by weight) comprising an anionic detergent surfactant (selected from one group of linear, branched, or randomly chained substituted or unsubstituted alkyl sulfates, alkyl sulfonates, alkyl alkoxylated sulfates, alkyl phosphates, alkyl phosphonates, alkyl carboxylates and / or mixtures thereof) and optionally a nonionic surfactant (selected from one group of linear, branched, or randomly chained substituted or unsubstituted alkyl alkoxylated alcohols, e.g., C8-C18 alkyl ethoxylated alcohols and / or C6-C12 alkylphenol alkoxylates), where the weight ratio of the anionic detergent surfactant (having a hydrophilicity index (HIc) of 6.0 to 9) to the nonionic detergent surfactant is greater than 1:1. Suitable detergent surfactants include cationic detergent surfactants (selected from the group consisting of alkylpyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, alkyl ternary sulfonium compounds and / or mixtures thereof); amphoteric and / or amphoteric detergent surfactants (selected from the group consisting of alkanolamine sulfobetaines); amphoteric surfactants; semipolar nonionic surfactants and mixtures thereof.

[0137] The detergents of this specification, such as strong laundry detergent compositions, may optionally include a surfactant-enhancing polymer consisting of an amphiphilic alkoxylated grease-cleaning polymer (selected from a group of branched hydrophilic and hydrophobic alkoxylated polymers, e.g., 0.05% to 10% by weight of alkoxylated polyalkylene imines) and / or a random graft polymer (typically consisting of a hydrophilic backbone comprising monomers selected from the group consisting of unsaturated C1-C6 carboxylic acids, ethers, alcohols, aldehydes, ketones, esters, sugar units, alkoxy units, saturated polyalcohols such as maleic anhydride and glycerol, and mixtures thereof; and hydrophobic side chains selected from the group consisting of C4-C25 alkyl groups, polypropylene, polybutylene, vinyl esters of saturated C1-C6 monocarboxylic acids, C1-C6 alkyl esters of acrylic acid or methacrylic acid, and mixtures thereof).

[0138] For example, the detergents of this specification, such as strong laundry detergent compositions, optionally include additional polymers, such as antifouling polymers (nonionic, end-capped polyesters, polymers comprising at least one monomer unit selected from saccharides, dicarboxylic acids, polyols and combinations thereof in random or block structures, such as SRP1, polymers based on ethylene terephthalate in random or block structures and copolymers thereof, such as REPEL-O-TEX SF, SF-2 and SRP6, TEXCARE SRA100, SRA300, SRN100, SRN170, SRN240, SRN300 and SRN325, MARLOQUEST The anti-re-adhesion agents specified herein (0.1% to 10% by weight) may include carboxylate polymers having molecular weights in the range of 500 to 100,000 Da, such as polymers comprising at least one monomer selected from acrylic acid, maleic acid (or maleic anhydride), fumaric acid, itaconic acid, aconitic acid, mesaconic acid, citraconic acid, methylenemalonic acid and any mixture thereof, vinylpyrrolidone homopolymer and / or polyethylene glycol; and polymer carboxylates (e.g., maleate / acrylate random copolymer or polyacrylate homopolymer).

[0139] For example, detergents of this specification, such as strong laundry detergent compositions, may optionally further contain saturated or unsaturated fatty acids, preferably saturated or unsaturated C12-C24 fatty acids (0% to 10% by weight); and deposition aids (examples of which include polysaccharides, cellulose polymers, polydiallyldimethylammonium halides (DADMAC) and copolymers of DAD MAC in random or block structures with vinylpyrrolidone, acrylamide, imidazole, imidazolium halides and mixtures thereof, cationic guar gum, cationic starch, cationic polyacrylamide and mixtures thereof).

[0140] For example, the detergents of this specification, such as strong laundry detergent compositions, optionally include dye transfer inhibitors, such as manganese phthalocyanine, peroxidase, polyvinylpyrrolidone polymer, polyamine N-oxide polymer, copolymer of N-vinylpyrrolidone and N-vinylimidazole, polyvinyloxazolidone and polyvinylimidazole and / or mixtures thereof, such as ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentamethylenephosphonic acid (DTPMP), hydroxyethanediphosphonic acid (HEDP), ethylenediamine N,N'-disuccinic acid (EDDS), methylglycinediacetic acid (MGDA), and diethylenetriaminepentaacetic acid (DTPMP). A) The chelating agents may include propylenediaminetetraacetic acid (PDTA), 2-hydroxypyridine-N-oxide (HPNO) or methylglycine diacetic acid (MGDA), N,N-diacetic acid (N,N-dicarboxymethylglutamate tetrasodium salt (GLDA)), nitrilotriacetic acid (NTA), 4,5-dihydroxy-m-benzenedisulfonic acid, citric acid and any salts thereof, N-hydroxyethylethylenediaminetriacetic acid (HEDTA), triethylenetetraaminehexaacetic acid (TTHA), N-hydroxyethyliminodiacetic acid (HEIDA), dihydroxyethylglycine (DHEG), ethylenediaminetetrapropionic acid (EDTP) and derivatives thereof.

[0141] For example, detergents of this specification, such as strong laundry detergent compositions, may optionally contain: a silicone or fatty acid-based soap foam inhibitor; a blurring dye, calcium and magnesium cations, visual signaling components, an antifoaming agent (0.001% to about 4.0% by weight); and / or a structural substance / thickener (0.01% to about 5% by weight) selected from the group consisting of diglycerides and triglycerides, ethylene glycol distearate, microcrystalline cellulose, microfiber cellulose, biopolymers, xanthan gum, gellan gum, and mixtures thereof. Such structural substances / thickeners will be included in the detergent in some embodiments, in addition to insoluble alpha-glucan particles. Structuring agents may also be called structural agents.

[0142] The detergents herein may, for example, be in the form of a strong drying / solid laundry detergent composition. Such detergents include (i) detergent surfactants, for example any anionic detergent surfactant disclosed herein, any nonionic detergent surfactant disclosed herein, any cationic detergent surfactant disclosed herein, any amphoteric and / or amphoteric detergent surfactant disclosed herein, any amphoteric surfactant, any semipolar nonionic surfactant and mixtures thereof; (ii) builders, for example any phosphate-free builders (e.g., zeolite builders in the range of 0% to less than 10% by weight), any phosphate builders (e.g., sodium tripolyphosphate in the range of 0% to less than 10% by weight), citric acid, citrates and nitrilotriacetic acid, any silicates (e.g., sodium silicate or potassium silicate or sodium metasilicate in the range of 0% to less than 10% by weight); any carbonates (e.g., sodium carbonate and / or sodium bicarbonate in the range of 0% to less than 80% by weight) and mixtures thereof; (i ii) Bleaching agents, such as photobleaching agents (e.g., zinc phthalocyanine sulfonate, aluminum phthalocyanine sulfonate, xanthene dyes and mixtures thereof), any hydrophobic or hydrophilic bleaching activators (e.g., dodecanoyloxybenzenesulfonate, decanoyloxybenzenesulfonate, decanoyloxybenzoic acid or salts thereof, 3,5,5-trimethylhexanoyloxybenzenesulfonate, tetraacetylethylenediamine-TAED, nonanoyloxybenzenesulfonate-NOBS, nitrile quat and mixtures thereof), any source of hydrogen peroxide (e.g., inorganic perhydrate salts, including mono or sodium tetrahydrate salts of perborate, percarbonate, persulfate, superphosphate or persilicate), any preforming hydrophilic and / or hydrophobic peracids (e.g., percarboxylic acids and salts, percarbonates and salts, perimide acids and salts, peroxomonosulfuric acid and salts and mixtures thereof);And / or (iv) any other components, such as bleaching catalysts (e.g., imine-based bleaching enhancers, including iminium cations and polyions, iminium amphoteric ions, modified amines, modified amine oxides, N-sulfonylimines, N-phosphonylimines, N-acylimines, thiadiazole dioxides, perfluoroimines, cyclic sugar ketones and mixtures thereof) and metal-containing bleaching catalysts (e.g., copper, iron, titanium, ruthenium, tungsten, molybdenum, or manganese cations, together with auxiliary metal cations such as zinc or aluminum and metal ion chelating agents such as EDTA, ethylenediaminetetra(methylenephosphonic acid)).

[0143] For example, detergents as specified herein, such as those for textile care (e.g., laundry), may be contained in unit doses (e.g., sachets or pouches). The form of a unit dose may include a water-soluble outer film that completely encloses the liquid or solid detergent composition. A unit dose may include a single compartment or at least two, three, or more compartments. The compartments may be arranged in an overlapping or side-by-side orientation. The unit doses as specified herein are typically enclosed structures of any form / shape suitable for retaining and protecting their contents without releasing the contents before contact with water.

[0144] The compositions disclosed herein may, for example, be in the form of dishwashing detergent compositions. Examples of dishwashing detergents include automatic dishwashing detergents (typically used in dishwashers) and hand-washing detergents. Dishwashing detergent compositions may, for example, be in any dry or liquid / aqueous form disclosed herein. Components that may be included in a particular embodiment of a dishwashing detergent composition include, for example, phosphates; oxygen-based or chlorine-based bleaches; nonionic surfactants; alkaline salts (e.g., metasilicates; alkali metal hydroxides, sodium carbonate); any active enzymes disclosed herein; rust inhibitors (e.g., sodium silicate); defoamers; additives for slowing the removal of gloss and patterns from ceramics; fragrances; anti-solidification agents (in granular detergents); starch (in tablet detergents); gelling agents (in liquid / gel detergents); and / or sand (in powder detergents).

[0145] For example, dishwashing detergents such as automatic dishwasher detergents or liquid dishwashing detergents contain (i) any ethoxylated nonionic surfactant, alkoxylated alcohol surfactant, epoxy-capped poly(oxyalkylated) alcohol or amine oxide surfactant present in an amount of 0 to 10% by weight; (ii) any phosphate builder (e.g., monophosphate, diphosphate, tripolyphosphate, other oligomeric polyphosphate, sodium tripolyphosphate-STPP) in an amount of approximately 5 to 60% by weight, any phosphate-free builder (e.g., methylglycine diacetic acid [MGDA] and their salts or derivatives, glutamine- Builders comprising N,N-diacetic acid [GLDA] and its salts or derivatives, iminodisuccinic acid (IDS) and its salts or derivatives, carboxymethyl inulin and its salts or derivatives, amino acid-based compounds including nitrilotriacetic acid [NTA], diethylenetriaminepentaacetic acid [DTPA], β-alaninediacetic acid [B-ADA] and their salts), homopolymers and copolymers of polycarboxylic acids and their partial or fully neutralized salts, monomer polycarboxylic acids and hydroxycarboxylic acids and their salts in the range of 0.5% to 50% by weight, or sulfonated / carboxylated polymers in the range of about 0.1% to about 50% by weight; (iii) 0.(iv) Drying aids in the range of 1% to about 10% by weight (e.g., polyesters, especially anionic polyesters, polycarbonates, polyurethanes, and / or polyureas, polyorganosiloxane compounds, or their particularly reactive cyclic carbonates and urea-type precursor compounds, together with monomers having optionally and 3 to 6 other functional groups—typically acid, alcohol, or ester functional groups that induce polycondensation); (iv) Silicates in the range of about 1% to about 20% by weight (e.g., sodium or potassium silicates, e.g., sodium disilicate, sodium metasilicate, and crystalline phyllosilicates); (v) Inorganic bleaches (e.g., perhydrate salts such as perborates, percarbonates, superphosphates, persulfates, and persilicates) and / or organic bleaches (e.g., diacyl and tetraacyl (vi) Organic peroxy acids such as peroxides, particularly diperoxide decanedioic acid and diperoxyhexadecanedioic acid; (vi) Bleaching activators (e.g., organic peracid precursors in the range of about 0.1% to about 10% by weight) and / or bleaching catalysts (e.g., manganese triazacyclononane and related complexes; Co, Cu, Mn, and Fe bispyridylamines and related complexes; and pentamine cobalt(III) acetate and related complexes); (vii) Metal care agents in the range of about 0.1% to 5% by weight (e.g., benzatriaazole, metal salts and complexes and / or silicates); and / or (viii) Any active enzymes disclosed herein in the range of about 0.01 to 5.0 mg per gram of the automatic dishwasher detergent composition, as well as enzyme stabilizers (e.g., oligosaccharides, polysaccharides, and inorganic divalent metal salts).

[0146] The detergents of this specification, such as those for the care of dishes, may be contained in, for example, a unit dose (e.g., a sachet or pouch) and may include a suitable dishwashing detergent composition, as described above with respect to textile care detergents.

[0147] The compositions disclosed herein may, for example, be in the form of oral care compositions. Examples of oral care compositions include toothpastes, toothpastes, mouthwashes, oral rinses, chewing gums and edible strips that provide some form of oral care (e.g., treatment or prevention of caries, gingivitis, plaque, tartar and / or periodontal disease). Oral care compositions may also be used to treat “oral surfaces,” which encompass all soft or hard surfaces in the oral cavity, including the surface of the tongue, the hard or soft palate, the buccal mucosa, the gums and tooth surfaces. In this specification, “tooth surfaces” refers, for example, to the surface of natural teeth or the hard surface of artificial teeth such as crowns, caps, fillings, bridges, dentures or dental implants.

[0148] The oral care compositions herein may, for example, contain about 0.01 to 15.0% by weight (e.g., about 0.1 to 10% by weight, about 0.1 to 5.0% by weight, or about 0.1 to 2.0% by weight) of the insoluble alpha-glucan particles disclosed herein. The insoluble alpha-glucan particles contained in the oral care compositions may sometimes be provided in the compositions as a thickener and / or dispersant, which may be useful in imparting the compositions a desired consistency and / or mouthfeel. The oral care compositions herein may also provide one or more other thickeners or dispersants, such as carboxyvinyl polymer, carrageenan (e.g., L-carrageenan), natural rubber (e.g., karaya, xanthan gum, acacia gum, tragacanth), colloidal magnesium aluminum silicate, or colloidal silica.

[0149] The oral care compositions herein may, for example, be toothpaste or other toothpastes. Such compositions herein and any other oral care compositions may, but are not limited to, further contain one or more of the following: caries preventive agents, antimicrobial or antimicrobial agents, anti-calculus or calculus preventive agents, surfactants, abrasives, pH adjusters, foaming agents, humectants, flavoring agents, sweeteners, pigments / colorants, whitening agents and / or other suitable ingredients. Examples of oral care compositions to which insoluble alpha-glucan particles may be added are disclosed in U.S. Patent Application Publications 2006 / 0134025, 2002 / 0022006 and 2008 / 0057007, which are incorporated herein by reference.

[0150] The caries prevention agents described herein may be orally acceptable sources of fluoride ions. Suitable sources of fluoride ions include, for example, fluorine compounds, monofluorophosphates and fluorosilicates, and amine fluorides, including olaflur (N'-octadecyltrimethylenediamine-N,N,N'-tris(2-ethanol)-dihydrofluoride). The caries prevention agent may be present in an amount that gives the composition a total of about 100 to 20,000 ppm, about 200 to 5,000 ppm, or about 500 to 2,500 ppm of fluoride ions. In oral care compositions where sodium fluoride is the sole source of fluoride ions, for example, sodium fluoride may be present in the composition in an amount of about 0.01 to 5.0% by weight, about 0.05 to 1.0% by weight, or about 0.1 to 0.5% by weight.

[0151] Suitable antimicrobial or antimicrobial agents for use in the oral care compositions of this specification include, for example, phenol compounds (e.g., 4-allylcatechol; p-hydroxybenzoic acid esters such as benzylparaben, butylparaben, ethylparaben, methylparaben, and propylparaben; 2-benzylphenol; butylated hydroxyanisole; butylated hydroxytoluene; capsaicin; carvacrol; creosol; eugenol; guaiacol; halogenated bisphenols such as hexachlorophene and bromochlorophene; salicylic acid esters such as 4-hexylresorcinol, 8-hydroxyquinoline and its salts, menthyl salicylate, methyl salicylate, and phenyl salicylate; phenol; pyrocatechol; salicylananilide; thymol; halogenated diphenyl ether compounds such as triclosan and triclosan monophosphate), copper(II) compounds (e.g., copper(II) chloride, fluoride, sulfate, and hydroxide), and zinc ion sources (e.g., zinc acetate, citrate, glycerol (conate, glycinate, oxides and sulfates), phthalic acid and its salts (e.g., magnesium monopotassium phthalate), hexetidine, octenidine, sanguinalin, benzalkonium chloride, domiphene bromide, alkylpyridinium chloride (e.g., cetylpyridinium chloride, tetradecylpyridinium chloride, N-tetradecyl-4-ethylpyridinium chloride), iodine, sulfonamides, bisbiguanides (e.g., alexidine, chlorhexidine, chlorhexidine gluconate), piperid Examples include derivatives of ion (e.g., dermopinol, octapinol), magnolia extract, grape seed extract, rosemary extract, menthol, geraniol, citral, eucalyptol, antibiotics (e.g., augumentin, amoxiline, tetracycline, doxycycline, minocycline, metronidazole, neomycin, kanamycin, clindamycin) and / or antimicrobial agents disclosed in U.S. Patent No. 5,776,435 (incorporated herein by reference). One or more antimicrobial agents may be optionally present in the disclosed oral care composition in amounts, for example, about 0.01 to 10% by weight (e.g., 0.1 to 3% by weight).

[0152] Suitable anti-calculus or calculus-preventing agents for use in the oral care compositions of this specification include, for example, phosphates and polyphosphates (e.g., pyrophosphates), polyaminopropanesulfonic acid (AMPS), zinc citrate trihydrate, polypeptides (e.g., polyaspartic acid and polyglutamic acid), polyolefin sulfonates, polyolefin phosphates, diphosphonates (e.g., azacycloalkane-2,2-diphosphonates such as azacycloheptane-2,2-diphosphonic acid), N-methylazacyclopentane-2,3-diphosphonic acid, ethane-1-hydroxy-1,1-diphosphonic acid (EHDP), ethane-1-amino-1,1-diphosphonate, and / or phosphonoalkane carboxylic acids and their salts (e.g., alkali metal salts and ammonium salts thereof). Examples of useful inorganic phosphates and polyphosphates include monobasic, dibasic, and tribasic sodium phosphates, sodium tripolyphosphates, tetrapolyphosphates, monosodium, disodium, trisodium, and tetrasodium pyrophosphates, disodium dihydrogen pyrophosphates, sodium trimetaphosphates, sodium hexamethaphosphates, or those in which the sodium is substituted with potassium or ammonium. Other useful anti-calculus agents in specific embodiments include anionic polycarboxylate polymers (e.g., polymers or copolymers of acrylic acid, methacrylic acid, and maleic anhydride, such as polyvinyl methyl ether / maleic anhydride copolymers). Further useful anti-calculus agents include metal ion chelating agents such as hydroxycarboxylic acids (e.g., citric acid, fumaric acid, malic acid, tartaric acid, and oxalic acid and their salts) and aminopolycarboxylic acids (e.g., EDTA). One or more anti-calculus agents or calculus inhibitors may be optionally present in the disclosed oral care composition in, for example, about 0.01 to 50% by weight (e.g., about 0.05 to 25% by weight or about 0.1 to 15% by weight).

[0153] Suitable surfactants for use in the oral care compositions described herein may be, for example, anionic, nonionic, or amphoteric. Suitable anionic surfactants include, but are not limited to, C 8~20 Water-soluble salts of alkyl sulfates, C 8~20Examples of fatty acid sulfonated monoglycerides, sarcosinates, and taurates include sodium lauryl sulfate, sodium coconut oil monoglyceride sulfonate, sodium lauryl sarcosinate, sodium lauryl isethionate, sodium laureth carboxylate, and sodium dodecylbenzenesulfonate. Suitable nonionic surfactants include, but are not limited to, poloxamers, polyoxyethylene sorbitan esters, fatty alcohol ethoxylates, alkylphenol ethoxylates, tertiary amine oxides, tertiary phosphine oxides, and dialkyl sulfoxides. Suitable amphoteric surfactants include, but are not limited to, C23 surfactants having an anionic group such as carboxylates, sulfates, sulfonates, phosphates, or phosphonates. 8~20 Examples include derivatives of secondary and tertiary aliphatic amines. An example of a suitable amphoteric surfactant is cocoamidopropyl betaine. One or more surfactants are optionally present in the disclosed oral care composition in a total amount of, for example, about 0.01 to 10% by weight (e.g., about 0.05 to 5.0% by weight or about 0.1 to 2.0% by weight).

[0154] Suitable abrasives for use in the oral care compositions herein include, for example, silica (e.g., silica gel, silicic acid, precipitated silica), alumina, insoluble phosphates, calcium carbonate, and resin abrasives (e.g., urea-formaldehyde condensation products). Examples of insoluble phosphates useful as abrasives herein are orthophosphates, polymetaphosphates, and pyrophosphates, including dicalcium orthophosphate dihydrate, calcium pyrophosphate, beta-calcium pyrophosphate, tricalcium phosphate, polymetaphosphate, and insoluble sodium polymetaphosphate. One or more abrasives are optionally present in the disclosed oral care compositions in a total amount of, for example, about 5 to 70% by weight (e.g., about 10 to 56% by weight or about 15 to 30% by weight). The average particle size of the abrasives in a particular embodiment is about 0.1 to 30 microns (e.g., about 1 to 20 microns or about 5 to 15 microns).

[0155] An oral care composition in a particular embodiment may include at least one pH modifier. Such an agent may be selected to acidify, make more basic, or buffer the pH of the composition to a pH range of about 2 to 10 (e.g., a pH range of about 2 to 8, 3 to 9, 4 to 8, 5 to 7, 6 to 10, or 7 to 9). Examples of pH modifiers useful herein, but not limited to, carboxylic acids, phosphonic acids and sulfonic acids; salts (e.g., monosodium citrate, disodium citrate, monosodium maleate); alkali metal hydroxides (e.g., carbonates and sesquicarbonates such as sodium hydroxide, sodium carbonate, sodium bicarbonate); borates; silicates; phosphates (e.g., monosodium phosphate, trisodium phosphate, pyrophosphate); and imidazoles.

[0156] Suitable foaming modifiers for use in the oral care compositions herein may be, for example, polyethylene glycol (PEG). For example, high molecular weight PEGs, including PEG having an average molecular weight of about 200,000 to 7,000,000 (e.g., about 500,000 to 5,000,000 or about 1,000,000 to 2,500,000), are suitable. One or more PEGs may be optionally present in the disclosed oral care compositions in a total amount of, for example, about 0.1 to 10% by weight (e.g., about 0.2 to 5.0% by weight or about 0.25 to 2.0% by weight).

[0157] An oral care composition in a particular embodiment may contain at least one humectant. The humectant in a particular embodiment may be glycerin, sorbitol, xylitol, or a polyhydric alcohol such as low molecular weight PEG. The most suitable humectant may also function as a sweetener as herein. One or more humectants may optionally be present in the oral care composition disclosed herein in a total amount of, for example, about 1.0 to 70% by weight (e.g., about 1.0 to 50% by weight, about 2 to 25% by weight, or about 5 to 15% by weight).

[0158] Natural or artificial sweeteners may be optionally included in the oral care compositions herein. Suitable sweeteners include dextrose, sucrose, maltose, dextrin, invert sugar, mannose, xylose, ribose, fructose, levose, galactose, corn syrup (e.g., high-fructose corn syrup or solid corn syrup), partially hydrolyzed starch, hydrolyzed starch, sorbitol, mannitol, xylitol, maltitol, isomalt, aspartame, neotame, saccharin and its salts, dipeptide-based strong sweeteners, and cyclamate salts. One or more sweeteners may be optionally present in the oral care compositions disclosed herein in a total amount, for example, about 0.005 to 5.0% by weight.

[0159] The oral care compositions of this specification may optionally contain natural or artificial flavorings. Suitable flavorings include vanillin; sage; marjoram; watercress oil; spearmint oil; cinnamon oil; wintergreen oil (methyl salicylate); peppermint oil; clove oil; bay oil; anise oil; eucalyptus oil; citrus oil; fruit oils; essential oils derived from lemon, orange, lime, grapefruit, apricot, banana, grape, apple, strawberry, cherry, or pineapple; flavorings derived from beans or nuts such as coffee, cocoa, cola, peanuts, or almonds; and adsorbent and encapsulating flavorings. Furthermore, the flavorings of this specification include components that provide aroma and / or other sensory effects in the mouth, including cooling or warming effects. Examples of such ingredients, but not limited to, include menthol, menthyl acetate, menthyl lactate, camphor, eucalyptus oil, eucalyptol, anethole, eugenol, cassia, oxanone, Irisone®, propenylguaetol, thymol, linalool, benzaldehyde, cinnamaldehyde, N-ethyl-p-menthane-3-carboxamine, N,2,3-trimethyl-2-isopropylbutanamide, 3-(1-menthoxy)-propane-1,2-diol, cinnamaldehyde glycerol acetal (CGA), and menthol glycerol acetal (MGA). One or more flavoring agents may be optionally present in the oral care compositions disclosed herein in a total amount, for example, about 0.01 to 5.0% by weight (e.g., about 0.1 to 2.5% by weight).

[0160] The oral care composition in a particular embodiment may contain at least one bicarbonate. For example, any orally acceptable bicarbonate can be used, including alkali metal bicarbonates such as sodium bicarbonate or potassium bicarbonate and ammonium bicarbonate. One or more bicarbonates may optionally be present in the oral care composition disclosed herein in a total amount, for example, about 0.1 to 50% by weight (e.g., about 1 to 20% by weight).

[0161] An oral care composition in a particular embodiment may contain at least one whitening agent and / or colorant. Suitable whitening agents are peroxides, such as those disclosed in U.S. Patent No. 8,540,971, which are incorporated herein by reference. Suitable colorants herein include, for example, chemicals that impart a particular gloss or reflectivity, such as pigments, dyes, lakes, and pearlants. Specific examples of useful colorants herein include talc; mica; magnesium carbonate; calcium carbonate; magnesium silicate; aluminum magnesium silicate; silica; titanium dioxide; zinc oxide; red, yellow, brown, and black iron oxides; ferric ammonium ferrocyanide compounds; manganese violet; ultramarine; titanized mica; and bismuth oxychloride. One or more colorants may optionally be present in an oral care composition disclosed herein in a total amount, for example, about 0.001 to 20% by weight (e.g., about 0.01 to 10% by weight or about 0.1 to 5.0% by weight).

[0162] Further components that may be optionally included in the oral care compositions herein include, for example, one or more enzymes (as described above), vitamins, and anti-adhesives. Examples of vitamins useful herein include vitamin C, vitamin E, vitamin B5, and folic acid. Examples of suitable anti-adhesives include sorbrol, ficin, and quorum sensing inhibitors.

[0163] This disclosure also relates to a method for processing the material. This method involves contacting the material with an aqueous composition containing insoluble alpha-glucan particles disclosed herein.

[0164] In some embodiments, the material to be brought into contact with the aqueous composition in the contact methods described herein may include textiles. The textiles described herein may include natural fibers, synthetic fibers, semi-synthetic fibers, or any combination thereof. The semi-synthetic fibers described herein are manufactured using chemically derivatized naturally derived materials, one example of which is rayon. Non-limiting examples of the types of fabrics described herein include: (i) cellulose fibers, such as cotton (e.g., broadcloth, canvas, chambray, chenille, chintz, corduroy, creton, damask, denim, flannel, gingham, jacquard, knit, materaze, oxford, percale, poplin, pristine, satin, seersucker, sheer, terrycloth, twill, velvet), rayon (e.g., viscose, modal, liocell), linen, and Tencel®; (ii) proteinaceous fibers, such as silk, wool, and related mammalian fibers; (iii) synthetic fibers, such as polyester, acrylic, nylon, etc.; (iv) plant filamentous fibers derived from jute, flax, ramie, coir, kapok, sisal, hennecken, abaca, hemp, and sunhemp; and (v) fabrics made from any combination of the fabrics of (i) to (iv). Textiles that include a combination of textile types (e.g., natural and synthetic) include, for example, textiles comprising both cotton fibers and polyester. Materials / articles containing one or more textiles of this specification include, for example, clothing, curtains, drapes, upholstery materials, carpets, bed linens, bath linens, tablecloths, sleeping bags, tents, and automotive interiors. Other materials containing natural and / or synthetic fibers include, for example, nonwovens, stuffings, paper, and foams.

[0165] The aqueous composition brought into contact with the fabric may be, for example, a fabric care composition (e.g., laundry detergent, fabric softener). Therefore, a processing method in a particular embodiment can be considered a fabric care method or a washing method if a fabric care composition is used therein. The fabric care compositions of this specification are thought to achieve one or more of the following fabric care benefits (i.e., substantial surface effects): wrinkle removal, wrinkle reduction, wrinkle resistance, reduced fabric abrasion, improved fabric abrasion resistance, reduced fabric pilling, extended fabric life, fabric color maintenance, reduced fabric fading, reduced dye migration, fabric color restoration, reduced fabric soiling, fabric soil shedding, fabric shape retention, enhanced fabric smoothness, prevention of soil re-adhesion on the fabric, prevention of graying of laundry, improved fabric texture / feel, and / or reduced shrinkage.

[0166] Examples of conditions (e.g., time, temperature, wash / rinse volume) for carrying out the textile care or washing methods specified herein are disclosed in International Publication No. 1997 / 003161 and U.S. Patents No. 4,794661, 4580421 and 5945394 (which are incorporated herein by reference). In other examples, materials including textiles are mixed with the aqueous compositions herein and (i) for at least about 5, 10, 20, 30, 40, 50, 60, 70, 80, 90, 100, 110 or 120 minutes; (ii) at at least about 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90 or 95°C (e.g., for washing or rinsing: at a “low” temperature of about 15–30°C, about It can be brought into contact at a "medium" temperature of 30-50°C or a "high" temperature of approximately 50-95°C; (iii) at a pH of approximately 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, or 12 (for example, a pH range of approximately 2-12 or approximately 3-11); (iv) at a salt (e.g., NaCl) concentration of at least approximately 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, or 4.0% by weight; or in any combination of (i) to (iv).

[0167] The contact step in a textile care or washing method may include, for example, a washing step, a soaking step, and / or a rinsing step. Further contact of a material or textile in another embodiment may be carried out by any means known in the art, such as dissolving, mixing, shaking, spraying, treating, soaking, flash washing, injecting onto or into, binding, painting, coating, applying, adding, and / or passing an effective amount of the insoluble alpha-glucan particles specified herein through the textile or material. In further embodiments, contact may be used to treat the textile to impart a substantial surface effect. As used herein, the terms “textile feel” or “touch” refer to an individual’s tactile sensory response to a textile, which may be physical, physiological, psychological, social, or any combination thereof. In one embodiment, the texture of a textile can be measured using a PHABROmeter® system (available from Nu Cybertek, Inc. Davis, CA) for measuring relative texture values ​​(as given by the American Association of Textile Chemists and Color Technicians [AATCC test method, “202-2012, Relative Hand Value of Textiles: Instrumental Method”]).

[0168] In some embodiments of processing materials including textiles, the insoluble alpha-glucan particle component of the aqueous composition adsorbs to the textile. This feature is thought to make the insoluble alpha-glucan particles herein useful as anti-redeposition and / or anti-graying agents (in addition to their viscosity-modifying effects) in the textile care compositions disclosed herein. The anti-redeposition or anti-graying agents herein help prevent dirt from re-adhering to clothing in the wash water after the dirt has been removed. Furthermore, the adsorption of the insoluble alpha-glucan particles herein to the textile may also enhance the mechanical properties of the textile.

[0169] The adsorption of insoluble alpha-glucan particles into the fabrics of this specification can be measured, for example, by colorimetric techniques (e.g., Dubois et al., 1956, Anal. Chem. 28:350-356; Zemljits et al., 2006, Lenzinger Berichte 85:68-76; both of these are incorporated herein by reference) or by any other method known in the art.

[0170] Other materials that can be brought into contact with the processing methods described above include surfaces that can be treated with dishwashing detergents (e.g., automatic dishwasher detergents or hand dishwashing detergents). Examples of such materials include the surfaces of plates, glasses, pots, pans, gratin dishes, cookware, and tableware (collectively referred to herein as “dishware”) made of ceramic materials, porcelain, metal, glass, plastics (e.g., polyethylene, polypropylene, polystyrene, etc.), and wood. Thus, the processing methods in particular embodiments can be considered, for example, as dishwashing methods or dishwashing cleaning methods. Examples of conditions (e.g., time, temperature, washing volume) for carrying out the dishwashing methods or dishwashing cleaning methods described herein are disclosed in U.S. Patent No. 8,575,083, which is incorporated herein by reference. In other examples, tableware products can be brought into contact with the aqueous compositions described herein under a suitable set of conditions, such as any of the conditions disclosed above with respect to contacting materials, for example, textiles.

[0171] Other materials that can be brought into contact with the treatment method described above include oral surfaces such as soft or hard surfaces in the oral cavity, including the tongue, hard and soft palate, buccal mucosa, gingiva, and tooth surfaces (e.g., natural teeth or the hard surfaces of artificial teeth such as crowns, caps, fillings, bridges, dentures, or dental implants). Therefore, the treatment method in a particular embodiment can be considered, for example, an oral care method or a dental treatment method. The conditions (e.g., time, temperature) for bringing the oral surface into contact with the aqueous composition of this specification must be suitable for the intended use in which such contact is made. Other surfaces that can be brought into contact with the treatment method include surfaces of the outer layer, such as skin, hair, or nails.

[0172] Accordingly, specific embodiments of this disclosure relate to materials (e.g., textiles) containing the insoluble alpha-glucan particles of this specification. Such materials can be produced, for example, according to the material processing methods disclosed herein. In some embodiments, the materials may contain insoluble alpha-glucan particles when the compound is adsorbed onto the surface of the material or in contact with other materials.

[0173] Certain embodiments of the methods for processing materials according to this specification further include a drying step of drying the material after contact with an aqueous composition. The drying step can be carried out immediately after the contact step or after one or more additional steps that may follow the contact step (e.g., washing in the aqueous composition according to this specification, then rinsing with water, and then drying the fabric). Drying can be carried out by several arbitrary means known in the art, such as air drying (e.g., about 20-25°C) or at temperatures of at least about 30, 40, 50, 60, 70, 80, 90, 100, 120, 140, 160, 170, 175, 180 or 200°C. The dried materials according to this specification typically contain less than 3, 2, 1, 0.5 or 0.1% by weight of moisture in the material. Fabrics are preferred materials for optionally carrying out the drying step.

[0174] The aqueous composition used in the processing method herein may be any of the aqueous compositions disclosed herein. Examples of aqueous compositions include detergents (e.g., laundry detergents or dish soaps), fabric softeners, and water-containing toothpastes such as toothpaste.

[0175] In some embodiments, the material that can be treated with a liquid composition comprising the insoluble alpha-glucan particles herein is a nonwoven fabric product. This treatment, which typically involves the application of an aqueous or non-aqueous composition (e.g., a dispersion) comprising the insoluble alpha-glucan particles herein (at any concentration disclosed herein) and a subsequent drying step (e.g., air drying, heat drying, vacuum drying; the drying temperature may be any suitable temperature disclosed herein), can strengthen the nonwoven fabric product (i.e., act as a binder for the nonwoven fabric product). In some embodiments, the insoluble alpha-glucan particles can increase the dry or wet tensile strength of the nonwoven fabric (measured at N / 5cm) by, for example, about or at least about 1000%, 10000%, 100000%, or 1000000%. Thus, nonwoven fabric products containing a binder / reinforcement comprising the insoluble alpha-glucan particles herein are further provided herein. Optionally, such insoluble alpha-glucan particles are crosslinkable; crosslinking agents and / or procedures disclosed herein (e.g., glyoxal, citric acid, PAE) may be used to prepare crosslinked glucan particles before applying them to nonwoven products. In some embodiments, the dry or wet tensile strength of a nonwoven containing the alpha-glucan binder herein may be about or at least about 10, 15, 20, 25, 50, 75, 100, 125, 130, 135, 140, 145, 150, 10-150, 15-150, 20-150, 25-150, 10-140, 15-140, 20-140, or 25-140 N / 5cm. Based on the total weight of the nonwoven material and alpha-glucan binder in the nonwoven product, the alpha-glucan content therein may be about 5, 10, 15, 20, 25, 5-25, 5-20, 10-25, or 10-20% by weight. In embodiments in which a crosslinking agent is used, it may be about 1, 2, 3, 4, 5, 6, 2-6, 2-5, 3-6, or 3-5% by weight of the total weight of the nonwoven product. The nonwoven products specified herein may be, for example, airlaid, drylaid, wetlaid, carded, electrospun, spunlace, spunbond, or meltblown.In some embodiments, nonwoven fabric products may include abrasive or sculpting sheets, agricultural coverings, agricultural seed strips, garment linings, automotive headliners or covers, aprons, cheese wraps, civil engineering fabrics, coffee filters, cosmetic removers or applicators, detergent pouches / sachets, fabric softener sheets, envelopes, face masks, filters, garment bags, thermal or electrical conductive fabrics, household care wipes (e.g., for floor care, hard surface cleaning, pet care, etc.), house wraps, hygiene products (e.g., sanitary pads / napkins, underpads), insulating materials, labels, laundry aids, medical care or personal injury care products (e.g., band-aids, cast padding or covers, dressings, packs, sterile packaging materials, sterile packaging, surgical drapes, surgical gowns, cotton swabs), mops, napkins or paper towels, paper, personal wipes or baby wipes, reusable bags, roofing undercovers, table linens, tags, tea or coffee bags, covers, vacuum cleaning bags, or wallpaper. The fibers of the nonwoven product may, in some embodiments, contain cellulose and / or alpha-1,3-glucan, or may contain one or more other materials disclosed herein that can be used to form fibers. Examples of nonwoven products, nonwoven product materials and / or methods for manufacturing nonwoven products and materials herein may be as disclosed in International Patent Application Publication No. 2019055397 or in U.S. Patent Application Publication Nos. 2018 / 0282918, 2017 / 0167063, 2018 / 0320291 or 2010 / 0291213, which are incorporated herein by reference.

[0176] For example, the compositions comprising insoluble alpha-glucan particles as described herein may be films or coatings. In some embodiments, the films or coatings may be dry films or coatings containing, for example, less than about 3, 2, 1, 0.5, or 0.1% by weight of water. In some embodiments, the films or coatings may contain about 20-40, 20-35, 20-30, 25-40, 25-35, or 25-30% by weight of insoluble alpha-glucan particles, with the remainder of the material optionally being water, aqueous solutions, and / or plasticizers. The amount of insoluble alpha-glucan particles contained in the film or coating of the present invention is, for example, about or at least about 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, It may be 46, 47, 48, 49, 50, 51, 52, 53, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, 99.5 or 99.9% by weight.

[0177] The films or coatings of this specification may have a thickness of, for example, about, at least about or at most about 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 2, 2.5, 5, 7.5, 10, 15.5, 15, 17.5, 20, 22.5, 25, 30, 35, 40, 45, 50, 75, 100, 150, 200, 0.5-1.5, 0.8-1.5, 1.0-1.5, 0.5-1.4, 0.8-1.4 or 1.0-1.4 mils (1 mil = 0.001 inches). In some embodiments, such thickness is uniform, which can be characterized by (i) being at least 20%, 30%, 40%, or 50% of the entire area of ​​the film / coating and (ii) having a continuous area with a standard deviation of thickness less than about 0.06, 0.05, or 0.04 mils. In some embodiments, the films or coatings herein can be characterized as thin (e.g., <2 mils). The films herein are typically cast films.

[0178] The films or coatings described herein may exhibit a variety of desired transparencys. For example, a film / coating may have high transparency (e.g., high light transmittance and / or low haze). When used in the present invention, light transmittance can refer to a film or coating that gives, for example, a light transmittance of at least about 10-99% or at least about 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, or 99% and / or a haze of less than 30%, 25%, 20%, 15%, 10%, 5%, 2.5%, 2%, or 1%. High light transmittance can optionally refer to a film / coating having at least about 90% light transmittance and / or a haze of less than 10%. The light transmittance of the films / coatings described herein can be measured, for example, according to the ASTM D1746 test (2009, Standard Test Method for Transparency of Plastic Sheeting, ASTM International, West Conshohocken, PA), which is incorporated herein by reference. The haze of the films / coatings described herein can be measured, for example, according to the ASTM D1003-13 test (2013, Standard Test Method for Haze and Luminous Transmittance of Transparent Plastics, ASTM International, West Conshohocken, PA), which is incorporated herein by reference.For example, the films / coatings of this specification having approximately 20-40, 20-35, 20-30, 25-40, 25-35, or 25-30% by weight of insoluble alpha-glucan particles (e.g., the remainder being water or an aqueous solution) have high light transmittance (e.g., >90% light transmittance and / or less than 10% haze), while other films / coatings having the same amount of insoluble alpha-glucan with DPw > 200 (e.g., DPw ≥ approximately 700 or approximately 800), crystallinity < 0.65 (e.g., ≤ 0.60), and / or a D50 diameter of 5-50 microns (e.g., unhydrolyzed) do not typically exhibit this beneficial characteristic (e.g., the latter type of film / coating may be hazy).

[0179] The films or coatings herein may optionally further contain plasticizers such as glycerol, propylene glycol, ethylene glycol, and / or polyethylene glycol. In some embodiments, other film components (in addition to the insoluble alpha-glucan particles herein) may be as disclosed in U.S. Patent Application Publication No. 2011 / 0151224, No. 2015 / 0191550, or No. 20190153674, U.S. Patent No. 9688035, No. 3345200, or International Publication No. 2018 / 200437, all of which are incorporated herein by reference.

[0180] In some embodiments, the films or coatings or suitable solid compositions of this specification may further comprise at least one crosslinking agent (e.g., composites). The insoluble alpha-glucan particles in the composition are crosslinkable (covalently) with each other and / or with at least one other component of the composition (e.g., polymer, surfactant) or, if the composition is applied to a substrate, with a component of the substrate. Furthermore, in some embodiments, the insoluble alpha-glucan particles do not crosslink in any way, but one or more other components of the composition do. Crosslinking can, for example, (i) increase the tensile strength of the film or coating composition and / or (ii) make it plastic. In some embodiments, crosslinking can crosslink the film or coating to a substrate. In some cases, crosslinking agents such as di- or polycarboxylic acids, aldehydes or polyphenols can be used to impart plasticity and crosslinking characteristics to the substrate. Suitable crosslinking agents for preparing the crosslinked compositions of this specification as described above include phosphoryl chloride (POCl3), polyphosphates, sodium trimetaphosphate (STMP), boron-containing compounds (e.g., boric acid, diborate, tetraborate, e.g., tetraborate decahydrate, pentaborate, polymer compounds, e.g., Polybor®, alkaliborate), polyvalent metals (e.g., titanium-containing compounds, e.g., titanium ammonium lactate, titanium triethanolamine, titanium acetylacetonate, or titanium polyhydroxy complexes; zirconium-containing compounds, e.g., zirconium lactate, zirconium carbonate) It is believed that the following substances are included: zinc, zirconium acetylacetonate, zirconium triethanolamine, zirconium diisopropylamine lactate, or zirconium polyhydroxy complexes), glyoxal, glutaraldehyde, aldehydes, polyphenols, divinyl sulfone, epichlorohydrin, polyamide-epichlorohydrin (PAE), di- or polycarboxylic acids (e.g., citric acid, malic acid, tartaric acid, succinic acid, glutaric acid, adipic acid), dichloroacetic acid, polyamines, diethylene glycol dimethyl ether (diglym), and ethylene glycol diglycidyl ether (EGDE).Further examples of suitable crosslinking agents are described in U.S. Patent Nos. 4,462,917, 4,464,270, 4,477,360, and 4,799,550, and U.S. Patent Application Publication No. 2008 / 0112907 (all of which are incorporated herein by reference). Furthermore, in some embodiments, the crosslinking agent is not a boron-containing compound (e.g., as described above). The insoluble alpha-glucans herein can be crosslinked by any of the crosslinking agents as otherwise disclosed herein, for example, in addition to films or coatings (e.g., in dispersions or other compositions disclosed herein).

[0181] To enhance the haptics of a film or coating, for example, one or more conditioning agents may be included in the film of the coating. The conditioning agents may be anionic emollients, e.g., sulfated oils, soaps, sulfated alcohols and / or oil emulsions; cationic emollients, such as quaternary ammonium compounds; nonionic emollients, such as polyoxyethylene derivatives, polyethylene emulsions, wax emulsions and / or silicon emollients; natural fatty acids; oils; monoglycerides; diglycerides; polyglycerides; citrate esters; lactic acid esters; and / or sugar esters, e.g., sucrose esters and / or sorbitan esters. Articles comprising adhesives, films, coatings or binders containing the insoluble alpha-glucan particles of this specification in a dry form are also disclosed. Such articles (optionally, “coated articles”) include a substrate having at least one surface on which the coating, adhesive, film or binder is arranged / deposited, in a substantially continuous or discontinuous manner. In some embodiments, the articles include paper, leather, wood, metal, polymers, fibrous materials, masonry, drywall, gypsum and / or building surfaces. “Building surface” as used herein refers to the exterior or interior surface of a building or other artificial structure. In some embodiments, the articles include porous substrates such as paper, cardboard, paperboard, corrugated cardboard, cellulose substrates, textiles or leather. Furthermore, in some embodiments, the articles may include polymers such as polyamides, polyolefins, polylactic acid, polyethylene terephthalate (PET), poly(trimethylene terephthalate) (PTT), aramids, polyethylene sulfide (PES), polyphenylene sulfide (PPS), polyimide (PI), polyethyleneimine (PEI), polyethylene naphthalate (PEN), polysulfone (PS), polyetheretherketone (PEEK), polyethylene, polypropylene, poly(cyclic olefin), poly(cyclohexylene dimethylene terephthalate), poly(trimethylene flange carboxylate) (PTF) or cellophane. In some embodiments, articles containing a fibrous base material include fibers, yarns, fabrics, fabric blends, textiles, nonwovens, paper, or carpets.The fibrous base material may contain natural and / or synthetic fibers such as cotton, cellulose, wool, silk, rayon, nylon, aramid, acetate, polyurethane urea, acrylic, jute, sisal, seaweed, coir, polyamide, polyester, polyolefin, polyacrylonitrile, polypropylene, polyaramid, or blends thereof.

[0182] The films, coatings, or other compositions (e.g., composites) described herein may, in some embodiments, have grease / oil and / or oxygen barrier properties. Such compositions may, together with the insoluble alpha-glucan particles described herein, contain one or more components as disclosed in U.S. Patent Application Publication No. 20190153674 or International Publication No. 2018 / 200437 (these are incorporated herein by reference). For example, the films, coatings, or other compositions herein may optionally contain, as a binder, one or more of the following: polyvinyl alcohol, polyvinyl acetate, partially saponified polyvinyl acetate, silanol-modified polyvinyl alcohol, butenediol vinyl alcohol copolymer (BVOH), polyurethane, starch, corn dextrin, carboxymethylcellulose, cellulose ether, hydroxyethylcellulose, hydroxypropylcellulose, ethyl hydroxyethylcellulose, methylcellulose, alginate, sodium alginate, xanthan gum, carrageenan, casein, soy protein, guar gum, synthetic polymers, styrene butadiene latex, and / or styrene acrylate latex. In some embodiments, compositions for preparing films, coatings, or other compositions may comprise about 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 65-85, 65-80, 70-85, or 70-80% by weight of a binder or compound such as polyvinyl alcohol (or any other compound referred to above) and about 50, 45, 40, 35, 30, 25, 20, 15, 10, 5, 2.5, 15-35, 20-35, 15-30, or 20-30% by weight of insoluble alpha-glucan particles disclosed herein. In some embodiments, compositions for preparing films, coatings, or other compositions may include a ratio of binder or compound (e.g., any of the compounds referenced above, such as polyvinyl alcohol or starch) to the insoluble alpha-glucan herein, based on the weight percent of each of these components in the composition, of about 7:3, 7.5, 2.5, 8:2, 8.5:1.5, or 9:1.In some embodiments, the films, coatings, or other compositions are starch-free, although in other embodiments, such as oxygen barriers, they may contain starch (as disclosed, for example, in U.S. Patent Application Publication No. 2011 / 0135912, or U.S. Patent No. 5621026, or U.S. Patent No. 6692801, all of which are incorporated herein by reference). The grease / oil barrier properties of the coatings or film compositions herein can be evaluated using a standard "KIT" type test, for example, according to the Technical Association of the Pulp and Paper Industry (TAPPI) Test Method T-559 cm-02 (Grease resistance test for paper and paperboard, TAPPI Press, Atlanta, GA, USA; incorporated herein by reference). In this test, good grease / oil barrier / resistance function is indicated by a value closer to 12 on a scale of 1 to 12. Grease / oil barrier properties and water / aqueous liquid barrier properties can be evaluated by the Cobb test disclosed in Example 8, if necessary. The barriers typically have Cobb index values ​​of 20, 17.5, 15, 12.5, 10, 7.5, or less than 5, as specified herein. The Cobb index values ​​of barriers with one or more of the compounds referenced above and the insoluble alpha-glucans specified herein may be about or at least about 10%, 20%, 30%, 40%, 50%, or 60% lower than, for example, the Cobb index values ​​of identical barriers without the insoluble alpha-glucans. The oxygen barrier properties of the coatings or film compositions specified herein can be evaluated by measuring the oxygen permeability rate (OTR) of the coatings.OTR can be determined, for example, according to ASTM F-1927-07 (2007, Standard Test Method for Determination of Oxygen Gas Transmission Rate, Permeability and Permeance at Controlled Relative Humidity Through Barrier Materials Using a Coulometric Detector, ASTM International, West Conshohocken, PA), which is incorporated herein by reference. OTR can be determined, for example, under relative humidity conditions of about 50% to 80%, 30% to 55%, 35% to 50%, or 30% to 80% and / or under temperatures of about or at least about 15, 20, 25, 30, 35, 40, 45, 15 to 40, 15 to 35, 15 to 30, 15 to 25, 20 to 40, 20 to 35, 20 to 30%, or 20 to 25°C. Examples of substrates herein that can utilize grease / oil and / or oxygen barrier coatings include any of the above substrates / surfaces, including cellulose (e.g., paper, cardboard, corrugated cardboard, textiles), polyethylene, polypropylene, polylactic acid, poly(ethylene terephthalate) (e.g., MYLAR), poly(trimethylene terephthalate), polyamide, polybutylene succinate, polybutylene adipate terephthalate, polybutylene succinate adipate, poly(trimethylene flange carboxylate), synthetic and / or petroleum-based or bio-based substrates. The grease / oil and / or oxygen barrier activity of coated materials herein may be increased by, for example, about or at least about 5%, 10%, 15%, or 20% compared to the grease / oil and / or oxygen barrier activity of materials containing a different coating from the above coating by (i) being uncoated or (ii) not containing insoluble alpha-glucan particulate components. Any of the above films, coatings, or other compositions may be, for example, in the form of laminates or extruded articles, and may be optionally positioned on any of the above substrates.

[0183] Films, coatings, or other compositions (e.g., dispersions, foams, masterbatches) containing the insoluble alpha-glucan particles herein may, in some embodiments, further comprise polyurethane (e.g., any of those disclosed herein). Such compositions may comprise, for example, about 1, 5, 10, 15, 20, 35, 30, 35, 40, 45, 50, 55, 60, 5-60, 5-50, 5-45, 5-40, 5-35, 5-30, 10-60, 10-50, 10-45, 10-40, 10-35, or 10-30% by weight of the insoluble alpha-glucan herein, with the remainder being the majority (e.g., 90% or 95% or more) consisting of one or more polyurethanes. Such compositions may be wet-form (e.g., dispersions of glucan and polyurethane) or dry-form (e.g., masterbatches, films / coatings, laminates, foams, or extruded composites of glucan and polyurethane). Polyurethanes as used herein may have molecular weights of, for example, about or at least about 1000, 1500, 2000, 2500, 3000, 3500, 4000, 1000-3000, 1500-3000, 1000-2500, or 1500-2500. Such compositions are subject to hydrolytic aging in some examples (e.g., exposure to 45-55 or about 50°C and / or 90-98% or about 95% relative humidity for 2-4 or 3 days). Polyurethane films, coatings, or other compositions as used herein may have any of the characteristics / values ​​listed in, for example, Tables 9 and 10 below (Example 10) (e.g., tensile stress at break, elongation at break %, tensile stress at 50% elongation, tensile stress at 300% elongation, area under the curve), or within plus / minus 5% or 10% thereof.In some embodiments, the polyurethane compositions having insoluble alpha-1,3-glucan according to this specification are heat and / or pressure workable, and the application of heat and / or pressure for compression molding, molding, extrusion molding or any other related processing step may be, for example, about or at least about 90, 95, 100, 105, 110, 115, 120, 130, 140, 95-115 or 100-110°C and / or pressures of at least about 5000, 10000, 15000, 20000 or 25000 psi. Such application of heat and / or pressure may be, for example, at least about 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 15 or 30 minutes. Compression-molded polyurethane compositions in some embodiments, such as films, may be about or at least about 70%, 75%, 80%, 85%, 90%, 95%, 98%, 99%, or 100% transparent or translucent. In some embodiments, any polyurethane composition disclosed herein may be produced by a process comprising providing an aqueous polyurethane dispersion and mixing the insoluble alpha-glucan particles specified herein with the polyurethane dispersion (e.g., by adding an aqueous dispersion of glucan particles). The resulting aqueous dispersion may be used directly to produce a composition (e.g., a film or a coating), or it may be dried into a masterbatch subsequently used to prepare the composition (e.g., by melt-processing).

[0184] In some embodiments, films or coatings may take the form of edible films or coatings. Such materials may, in some embodiments, include the insoluble alpha-glucan particles as described herein and one or more components described in U.S. Patent No. 4,710,228, No. 4,543,370, No. 4,820,533, No. 4,981,707, No. 5,470,581, No. 5,997,918, No. 8,206,765, or No. 8,999,413, or U.S. Patent Application Publication 2005 / 0214414 (these documents are incorporated herein by reference). In some embodiments, the insoluble alpha-glucan particles optionally replace starch and / or starch derivatives in edible films or coatings disclosed in any of the above references. Edible films or coatings may be used on, for example, potato products (e.g., potato flakes such as French fries), other vegetables or vegetable products (e.g., fresh cuts of any of zucchini, pumpkin, sweet potato, onion, okra, pepper, green bean, tomato, cucumber, lettuce, cabbage, carrot, broccoli, cauliflower, Brussels sprouts, bean sprouts, onion, or any of the vegetables), mushrooms, fruits (e.g., berries, e.g., raspberries, strawberries or blueberries, avocado, kiwi, kumquat, orange, tangerine, apple, pear, banana, grapefruit, cherry, papaya, lemon, lime, mango, peach, cantaloupe, or any of the fruits, or fresh cuts of the fruit) and / or nuts (peanuts, walnuts, almonds, pecans, cashews, hazelnuts, Brazil nuts, macadamia nuts). For example, where appropriate, any other food products disclosed herein may have an edible coating. These and other food products having edible films or coatings herein may, in some embodiments, be fried or baked, and / or the films or coatings may provide softness, moisture retention, protection from moisture, crispness, dietary fiber (instead of digestible starch), oxygen barrier, freshness, and / or anti-ripening properties.In some embodiments, anti-ripening properties can be measured by the degree to which the coating reduces the release of gaseous ripening hormones such as ethylene by plant products (e.g., at 15-30, 15-25, or 20-25°C) by (e.g., at least 25%, 50%, 75%, 80%, 85%, or 90%) and / or the degree to which the coating reduces the softening and / or sweetening of plant products. Edible coatings in some embodiments can be prepared by applying an aqueous dispersion of the insoluble alpha-glucan specified herein (e.g., in water or aqueous solution at 5-15%, 5-12%, 5-10%, 7.5-15%, 7.5-12%, or 7.5-10% by weight) to food and drying the dispersion (e.g., by air drying, forced air drying, vacuum drying, and / or heating).

[0185] In some embodiments, coating compositions that can be used to prepare the coatings of this specification may include any of the above components / materials / formulations. In some embodiments, the coating composition is a latex composition such as those described below.

[0186] The compositions comprising insoluble alpha-glucan particles as described herein may be latex compositions. Examples of latex compositions as described herein include paints (e.g., primers, finishes / decoratives), adhesives, films, coatings, and binders. The formulations and / or components of the latex compositions as described herein (in addition to the insoluble alpha-glucan particles as described herein) may be as described, for example, in U.S. Patent Nos. 6,881,782, 3,440,199, 3,294,709, 5312,863, 4069,186, and 6297,296, and International Publication No. 2019046123 (all of which are incorporated herein by reference).

[0187] The insoluble alpha-glucan particles disclosed herein are, based on the weight of all dispersed polymer solids in the latex, present in amounts of about or at least about 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, It may be present in the latex composition in any useful amount such as 0.9%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 15%, 20%, 25%, 30%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 0.01%~75%, 0.01%~5%, 5%~20%, 20%~50%, or 50%~75%.

[0188] Some embodiments of latex compositions may include polymers polymerized from at least one ethylene-unsaturated monomer (e.g., monoethylene-unsaturated monomer); polyurethanes; epoxy and / or rubber elastomers. Examples of monoethylene-unsaturated monomers herein include vinyl monomers, acrylic monomers, allyl monomers, acrylamide monomers, monocarboxyl unsaturated acids and dicarboxyl unsaturated acids.

[0189] Suitable vinyl monomers for polymers in the latex compositions herein include any compound having vinyl functionality (i.e., ethylene unsaturated), such as vinyl esters (e.g., vinyl acetate, vinyl propionate, vinyl laurate, vinyl pivalate, vinyl nonanoate, vinyl decanoate, vinyl neodecanoate, vinyl butyrate, vinyl benzoate, isopropyl vinyl acetate), vinyl aromatic hydrocarbons (e.g., styrene, methylstyrene and similar lower alkylstyrenes, chlorostyrene, vinyltoluene, vinylnaphthalene, divinylbenzene), and vinyl aliphatic hydrocarbons (e.g., vinyl chloride; vinyl chloride Lydenes; alpha-olefins, e.g., ethylene, propylene, and isobutylene; conjugated dienes, e.g., 1,3-butadiene, methyl-2-butadiene, 1,3-piperylene, 2,3-dimethylbutadiene, isoprene, cyclohexene, cyclopentadiene, and dicyclopentadiene); and vinyl alkyl ethers (e.g., methyl vinyl ether, isopropyl vinyl ether, n-butyl vinyl ether, isobutyl vinyl ether) are included, but compounds having acrylic functionality (e.g., acrylic acid, methacrylic acid, esters of such acids, acrylonitrile, acrylamide) are excluded. In some embodiments, the latex compositions herein include vinyl acetate-ethylene copolymers, carboxylated vinyl acetate-ethylene copolymers, and / or polyvinyl acetates.

[0190] Suitable acrylic monomers for polymers in the latex compositions of this specification include alkyl acrylates, alkyl methacrylates, acrylate acids, methacrylates, aromatic derivatives of acrylic and methacrylic acids, acrylamides, and acrylonitriles. Typically, alkyl acrylate and methacrylate monomers (also called alkyl esters of acrylic acid or methacrylic acid) have an alkyl ester moiety containing 1 to about 18 carbon atoms or 1 to about 8 carbon atoms per molecule. Suitable acrylic monomers include, for example, methyl acrylate and methacrylate, ethyl acrylate and methacrylate, butyl acrylate and methacrylate, propyl acrylate and methacrylate, 2-ethylhexyl acrylate and methacrylate, cyclohexyl acrylate and methacrylate, decyl acrylate and methacrylate, isodecyl acrylate and methacrylate, benzyl acrylate and methacrylate, isobornyl acrylate and methacrylate, neopentyl acrylate and methacrylate, and 1-adamantyl methacrylate. If acidic functionality is desired, acids such as acrylic acid or methacrylic acid can also be used.

[0191] Some embodiments of latex compositions include polyurethane polymers. Suitable polyurethane polymers include polysaccharides, as disclosed in International Publication No. 2018 / 017789 (incorporated herein by reference). Polyurethane-containing latex can be prepared, for example, as disclosed in U.S. Patent Application Publication No. 2016 / 0347978 (incorporated herein by reference), and / or may comprise reaction products of one or more polyisocyanates and one or more polyols. Useful polyols include, for example, polycarbonate polyols, polyester polyols, and polyether polyols. The polycarbonate polyurethanes herein can be formed as reaction products of polyols, such as 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, or tetraethylene glycol, and diaryl carbonates, such as diphenyl carbonate or phosgene. At least one of the polyisocyanates in this specification may be an aliphatic polyisocyanate, an aromatic polyisocyanate, or a polyisocyanate having both an aromatic group and an aliphatic group.Examples of polyisocyanates include 1,6-hexamethylene diisocyanate, isophorone diisocyanate, 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, mixtures of 2,4- and 2,6-toluene diisocyanates, bis(4-isocyanatocyclohexyl)methane, 1,3-bis(1-isocyanato-1-methylethyl)benzene, bis(4-isocyanatophenyl)methane, 2,4'-diphenylmethane diisocyanate, 2,2'-diphenylmethane diisocyanate, 2,4-diisocyanatotoluene, bis(3-isocyanatophenyl)methane, 1,4-diisocyanatobenzene, 1,3-diisocyanato-o-xylene, 1,3-diisocyanato This includes -p-xylene, 1,3-diisocyanato-m-xylene, 2,4-diisocyanato-1-chlorobenzene, 2,4-diisocyanato-1-nitrobenzene, 2,5-diisocyanato-1-nitrobenzene, m-phenylenediisocyanate, hexahydrotoluene diisocyanate, 1,5-naphthalenediisocyanate, 1-methoxy-2,4-phenylenediisocyanate, 4,4'-biphenylmethane diisocyanate, 4,4'-biphenylenediisocyanate, 3,3'-dimethyl-4,4'-diphenylmethane diisocyanate, 3,3'-4,4'-diphenylmethane diisocyanate, and 3,3'-dimethyldiphenylmethane-4,4'-diisocyanate. Furthermore, polyisocyanate homopolymers containing, for example, allophanate, biuret, isocyanurate, iminooxadiazinedione, or carbodiimide groups are also useful herein.The polyols used herein include any polyols containing two or more hydroxyl groups, such as C2-C12 alkanediols, ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, isomers of butanediol, pentanediol, hexanediol, heptanediol, octanediol, nonanediol, decanediol, undecanediol, dodecanediol, 2-methyl-1,3-propanediol, 2,2-dimethyl-1,3-propanediol (neopentyl glycol), 1,4-bis(hydroxymethyl)cyclohexane, 1,2,3-propanetriol (glycerol), and 2-hydroxymethyl-2-methyl 1,3-propanol (trimethylolethane), 2-ethyl-2-hydroxymethyl-1,3-propanediol (trimethylolpropane), 2,2-bis(hydroxymethyl)-1,3-propanediol (pentaerythritol), 1,4,6-octanetriol; chloropentanediol; glycerol monoalkyl ether; glycerol monoethyl ether; diethylene glycol; 1,3,6-hexanetriol; 2-methylpropanediol; 2,2,4-trimethyl-1,3-pentanediol, cyclohexanedimethanol; polymer polyols, such as polyether polyols or polyester polyols. In some embodiments, the polyols herein may be poly(oxytetramethylene) glycol, polyethylene glycol, or poly1,3-propanediol. In some embodiments, the polyols may be polyester polyols, such as those produced by the transesterification reaction of aliphatic diacids with aliphatic diols. Suitable aliphatic diacids include, for example, C3-C10 diacids, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, and sebacic acid. In some embodiments, aromatic and / or unsaturated diacids can also be used to form polyester polyols.

[0192] Some embodiments of latex compositions include epoxy polymers / resins (polyepoxides), such as bisphenol A epoxy resin, bisphenol F epoxy resin, Novolac epoxy resin, aliphatic epoxy resin, or glycidylamine epoxy resin.

[0193] Some embodiments of latex compositions include rubber elastomers. In some embodiments, rubber elastomers include, for example, one or more diene-based sulfur vulcanizable elastomers having a glass transition temperature (Tg) of less than -30°C, as measured by dynamic mechanical analysis. In further examples, rubber elastomers as herein include, for example, natural rubber, synthetic polyisoprene, polybutadiene rubber, styrene / butadiene copolymer rubber, ethylene propylene diene monomer rubber, hydrogenated nitrile butadiene rubber, neoprene, styrene / isoprene / butadiene copolymer rubber, butadiene / acrylonitrile rubber, polyisoprene rubber, isoprene / butadiene copolymer rubber, nitrile rubber, ethylene-acrylic rubber, butyl and halobutyl rubber, chlorosulfonated polyethylene, fluoroelastomers, hydrocarbon rubber, polybutadiene and silicone rubber.

[0194] The latex compositions herein comprise insoluble alpha-glucan particles dispersed in a dispersion (in which other polymers, such as those mentioned above, may be optionally dispersed together with the alpha-glucan particles) or emulsion, and the liquid component of the latex may be water or an aqueous solution. Aqueous solutions of latex in some embodiments may contain organic solvents that are miscible with water or immiscible. Suitable organic solvents herein include acetone, methyl ethyl ketone, butyl acetate, tetrahydrofuran, methanol, ethanol, isopropanol, diethyl ether, glycerol ether, hexane, toluene, dimethylacetamide, dimethylformamide, and dimethyl sulfoxide.

[0195] The latex compositions of this specification may further include one or more additives in some embodiments. Examples of additives of this specification include dispersants, rheological aids, defoamers, foaming agents, adhesion promoters, flame retardants, bactericides, fungicides, preservatives, optical whitening agents, fillers, antiprecipitants, fusing agents, wetting agents, buffering agents, pigments / colorants (e.g., metal oxides, synthetic organic pigments, carbon black), viscosity modifiers, antifreezes, surfactants, binders, crosslinking agents, corrosion inhibitors, curing agents, pH adjusters, salts, thickeners, plasticizers, stabilizers, fillers, and matting agents. Examples of pigments of this specification include titanium dioxide (TiO2), calcium carbonate, diatomaceous earth, mica, hydrated aluminum oxide, barium sulfate, calcium silicate, clay, silica, talc, zinc oxide, aluminum silicate, nepheline syenite, and mixtures thereof. In some embodiments, the latex composition is essentially free of starch, starch derivatives (e.g., hydroxyalkyl starch), cellulose and / or cellulose derivatives (e.g., carboxymethylcellulose) (e.g., less than 1, 0.5, 0.1, or 0.01% by weight of any of these components).

[0196] The latex compositions in the form of paints or other colorants described herein may, in some embodiments, have a pigment concentration (PVC) ranging from about 3% to about 80%. For example, matte paints may have a PVC ranging from about 55% to 80%, primers or undercoats may have a PVC ranging from about 30% to 50%, and / or gloss colorants may have a PVC ranging from about 3% to 20%. Some embodiments of paints or other colorants may have a PVC of about 55%, 60%, 65%, 70%, 75%, 80%, 55-80%, 55-75%, 55-70%, 60-80%, 60-75%, 60-70%, 63-67%, 64-66%, 65-80%, 65-75%, or 65-70%. The PVC values ​​herein may be those of specific pigments (or mixtures of pigments), such as those disclosed above (e.g., titanium dioxide). It is noteworthy that the insoluble alpha-glucan particles of this disclosure can act as pigment extenders (see the following examples). For example, insoluble alpha-glucan particles can be used to replace a portion of the amount of pigment in a paint (e.g., to reduce the amount of pigment by about or at least about 1%, 2.5%, 5%, 7.5%, 10%, 12.5%, 15%, 17.5%, 20%, 22.5%, 25%, 27.5%, 30%, 5-15%, 5-20%, 5-25%, 5-30%, 10-15%, 10-20%, 10-25%, 10-30%, 15-20%, 15-25%, 15-30%), while at the same time optionally increasing the opacity of the paint by about or at least about 1%, 1.25%, 1.5%, 1.75%, 2%, 2.25%, 1-2.25%, 1-2%, or 1-1.75% (despite the reduced amount of pigment). The substitution of pigments with insoluble alpha-glucan particles as described herein can be based on, for example, about 0.9 to 1.1 parts (e.g., 1.0 parts) of pigment for about 0.5 to 0.7 parts (e.g., 0.6 parts) of insoluble alpha-glucan particles.Aside from these advantages (opacity, less pigment required), the insoluble alpha-glucan particles of the present disclosure are considered to provide latex compositions (for example, for use as paints or other colorants) with one or more of the following other physical properties: for example, increased hardness, reduced tackiness, reduced gloss (i.e., resulting in a matte effect), increased shear strength, better abrasion resistance, improved drying time, improved fade resistance, reduced blistering, and / or improved tactile feel (less tacky feel), compared to latex compositions that differ only in that they do not contain insoluble alpha-glucan particles.

[0197] The latex compositions herein can be applied to the substrate (above) of an article using any method known in the art. Typically, after application of the latex composition, at least a portion of the aqueous solution is removed, for example, by drying, to provide an adhesive, film, coating, or binder containing the latex composition in a dried or semi-dried form. Suitable application methods include air knife coating, rod coating, bar coating, wire bar coating, spray coating, brush coating, cast coating, flexible blade coating, gravure coating, jet applicator coating, short dwell coating, slide hopper coating, curtain coating, flexographic printing coating, size-press coating, reverse roll coating, and transfer roll coating. The latex composition may be applied to at least a portion of the substrate, for example, one or more coats / applications.

[0198] Some aspects of this specification relate to compositions containing pigments. Compositions containing pigments may be in a liquid state (e.g., aqueous or non-aqueous compositions as specified herein) or a solid state (e.g., dry compositions as specified herein). Examples of compositions containing pigments include any of the compositions disclosed in other parts of this specification (e.g., paints, primers, colorants), inks, dyes (e.g., food coloring dyes, textile coloring dyes), resins, sunscreens, and cosmetics (e.g., mascaras, blushes, nail varnishes / polishes, lipsticks, glosses, eyeliners, foundations, eyeshadows, skin decoration compositions). Compositions containing pigments may be in a liquid state (e.g., aqueous or non-aqueous compositions as specified herein) or a solid state (e.g., dry compositions as specified herein). The pigments in the compositions containing pigments may be, for example, any of the pigments specified herein. Examples of pigments for these and / or other embodiments of this Specification include oxides of titanium (e.g., titanium dioxide), zinc, iron, zirconium, cerium, and chromium; manganese violet; ultramarine blue; chromium hydrate; Prussian blue; zinc sulfide; nitroso, nitro, azo, xanthene, quinoline, anthraquinone, and / or phthalocyanine compounds; metal complex compounds; and isoindolinone, isoindoline, quinacridone, perinone, perylene, diketopyrrolopyrrole, thioindigo, dioxazine, triphenylmethane, and / or quinophthalone compounds. Further examples of pigments useful herein are disclosed in U.S. Patent Application Publication No. 2006 / 0085924 (incorporated herein by reference).

[0199] In some embodiments, compositions comprising insoluble alpha-glucan particles may take the form of composites (e.g., rubber composites or polyurethane composites) as disclosed, for example, in International Publication No. 2018 / 081263 or 2018 / 017789 or in U.S. Patent Application Publication No. 2019 / 0225737 and 2017 / 0362345 (all of which are incorporated herein by reference). Optionally, the composites disclosed herein may be shown to comprise at least one polymer in addition to the insoluble alpha-glucan particles. One or more of the above components of the latex composition (e.g., rubber or polyurethane) may optionally be additional polymers in such composites. The additional polymers in the composites of this specification may be any suitable polymer disclosed above with respect to rubber, polyurethane, thermoplastic polymer, polyethylene, polypropylene, ethylene copolymer, polyvinyl butyrate, polylactic acid, polyvinyl alcohol, polyamide, polyether thermoplastic elastomer, polyester, polyether ester, ethylene vinyl alcohol copolymer, starch, cellulose, or latex components.

[0200] Rubber in some embodiments may be, for example, one or more of natural rubber, synthetic rubber, polyisoprene, polybutadiene, styrene-butadiene copolymer, styrene-isoprene copolymer, butadiene-isoprene copolymer, styrene-butadiene-isoprene copolymer, ethylene propylene diene monomer rubber, hydrogenated nitrile butadiene rubber, silicone rubber, or neoprene. Examples of rubber composites according to this specification include tires (e.g., automobile / bicycle; pneumatic tires; including tire treads and / or sidewalls), belts (e.g., conveyor belts, power transmission belts), hoses, gaskets, footwear (e.g., shoes, sneakers, boots; soles, cushions and / or aesthetic features), coatings, films, and adhesives. The rubber composites according to this specification are typically vulcanized. In particular, incorporating the insoluble alpha-glucan particles specified herein into rubber-containing composites can provide advantages such as lower cost, lower density, lower energy consumption between processes, and / or better or equivalent performance (e.g., increased wet traction, reduced rolling resistance, lighter weight, and / or mechanical strength) compared to using existing fillers such as carbon black or silica; such performance enhancements may, in some embodiments, be due to the tire. In some embodiments, the insoluble alpha-glucan particles specified herein replace about or at least about 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, or 100% by weight of fillers (e.g., carbon black or silica) that are typically currently used in rubber composites such as tires. Note that rubber composite tires currently on the market (without the insoluble alpha-glucan particles specified herein) typically contain up to about 30% by weight of existing fillers such as carbon black. Accordingly, the rubber composites of this specification, such as tires, may contain, for example, about or at least about 5, 10, 15, 20, 25, or 30% by weight of insoluble alpha-glucan particles disclosed herein.The rubber compositions comprising insoluble alpha-glucan particles as described herein may, in some embodiments, have a low minimum elastic torque (ML) (e.g., about 0.10, 0.08, 0.06, 0.04, 0.03, or 0.02 dNm [decineuton-meter] or less), and methods for mixing the rubber compositions during their preparation are disclosed. The rubber compositions comprising insoluble alpha-glucan particles as described herein may have any of the characteristics / values ​​listed in Table 5 (Example 9) below (e.g., density, tensile strength, elongation, modulus, tandelta, curing time, elastic torque), or may be within plus / minus 5% or 10% thereof. The rubber compositions comprising insoluble alpha-glucan particles as fillers according to this specification may, for example, contain any of the other non-filler materials / components listed in Table 4 (Example 9) below (optionally within plus / minus 5% or 10% of the listed content) and / or may have the listed content of insoluble alpha-glucan particles (or plus / minus 5% or 10% thereof).

[0201] This disclosure also relates to compositions comprising at least two distinct phases and insoluble alpha-glucan particles as herein, wherein the particles are at the interface of the two phases. Typically, the particles can alter (e.g., decrease) the interfacial tension between the two phases. For example, one phase may be hydrophilic (e.g., water, aqueous solutions, or aqueous dispersions, or other aqueous compositions as herein), while the other phase may be hydrophobic (e.g., oils and / or other organic liquids). Although the insoluble alpha-glucan particles as herein are located at the interface of the two phases, the particles may also optionally reside in at least one of the different phases (e.g., hydrophilic phases). Interfacial tension can be measured in units of mN / m (millineutons per meter). In some embodiments, insoluble alpha-glucan particles can reduce the interfacial tension by approximately or at least approximately 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 25, 30, 35, 40, 5-30, 5-25, 5-20, 5-15, 5-10, 10-30, 10-25, 10-20, or 10-15 mN / m.

[0202] Non-limiting examples of compositions and methods disclosed herein include: 1a. A composition comprising insoluble alpha-glucan particles having a crystallinity of at least about 0.65, wherein the insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least 15, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds. 2a. The composition of Embodiment 1a, wherein at least about 90% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 bonds. 3a. The composition of Embodiment 1a, wherein at least about 99% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 bonds. 4a. The composition of Embodiment 1a, 2a, or 3a, wherein the DPw of the insoluble alpha-glucan is at least about 35 or 40, or about 35 or 40 to about 100. 5a. The composition of Embodiment 1a, 2a, or 3a, wherein the DPw of the insoluble alpha-glucan is about 35 or 40 to about 60. 6a. The composition of Embodiment 1a, 2a, 3a, 4a, or 5a, which is an aqueous composition (e.g., a dispersion, an emulsion). 7a. The aqueous composition is a dispersion of the composition of Embodiment 6a. 8a. The composition of Embodiment 7a, wherein insoluble alpha-glucan particles are dispersed throughout at least about 90% of the volume of the dispersion. 9a. The aqueous composition is the composition of Embodiment 6a, 7a, or 8a, having a pH of about 0.0 to about 5.0. 10a. The aqueous composition of Embodiment 6a, 7a, or 8a, having a pH of about 0.0 to about 1.0 or about 0.0 to about 2.0. 11a. The aqueous composition of Embodiment 6a, 7a, or 8a, having a pH of about 2.0 to about 4.0, and optionally this pH range provides the composition with an antimicrobial effect (e.g., killing or inhibiting the growth / proliferation of microorganisms such as bacteria, yeast, or algae). 12a. A composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a or 11a, wherein at least 70% by weight of insoluble alpha-glucan particles have a diameter of less than 1.0 micron. 13a. Compositions of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, or 11a, wherein 45 to 55% by weight of insoluble alpha-glucan particles have a diameter of less than 0.35 microns. 14a. The composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a or 13a, wherein the temperature of the composition is up to about 125°C. 15a. Compositions of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a or 14a, wherein the insoluble alpha-glucan particles have a crystallinity of at least about 0.7. 16a. A composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a, 14a or 15a, wherein at least 80% by weight of the particles are in the form of plates. 17a. Compositions of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a, 14a, 15a or 16a, which are household care products, personal care products, industrial products, ingestible products (e.g., food) or pharmaceuticals. 18a. A composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a, 14a, 15a, 16a or 17a, wherein (a) a latex composition such as a paint or adhesive; (b) a composition containing a pigment such as a paint or sunscreen; (c) a film or coating such as an edible film or coating; (d) a detergent composition; (e) a composite material comprising at least one polymer in addition to insoluble alpha-glucan particles, wherein the additional polymer is optionally polyurethane, rubber or a thermoplastic polymer; or (f) a capsule material for encapsulating a composition containing a compound, wherein the capsule material allows for controlled release of the compound. 19a. A composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a, 14a, 15a, 16a, 17a or 18a, further comprising at least one additive that modifies the mechanical properties of the composition, optionally the additive being selected from crosslinking agents, plasticizers, conditioning agents, dispersants or wetting agents, optionally further comprising a composition being a film or a coating. 20a. The composition of Embodiments 1a, 2a, 3a, 4a, 5a, 6a, 7a, 8a, 9a, 10a, 11a, 12a, 13a, 14a, 15a, 16a, 17a, 18a or 19a, comprising at least two different phases, wherein the insoluble alpha-glucan particles are located at the interface of the two different phases. 21a. A method for producing insoluble alpha-glucan particles (as described in any of embodiments 1a to 5a, 12a, 13a, 15a or 16a), comprising: (a) providing an insoluble alpha-glucan produced in an enzymatic reaction comprising at least water, sucrose, and a glucosyltransferase enzyme for synthesizing insoluble alpha-glucan, wherein the insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least about 200, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds; (b) hydrolyzing the insoluble alpha-glucan to insoluble alpha-glucan particles having a DPw of about 35 or 40 to about 100, the hydrolysis being carried out under aqueous conditions at a pH of 2.0 or less; and (c) optionally isolating the insoluble alpha-glucan particles produced in step (b).

[0203] Non-limiting examples of compositions and methods disclosed herein include: 1b. A composition comprising insoluble alpha-glucan particles, wherein at least 80% by weight of the particles are in the form of plates, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds, and (i) at least 70% by weight of the insoluble alpha-glucan particles have a diameter of less than 1.0 micron, and / or (ii) 45 to 55% by weight of the insoluble alpha-glucan particles have a diameter of less than 0.35 micron. 2b. The composition of claim 1b, wherein at least about 90% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 bonds. 3b. The composition of claim 1b, wherein at least about 99% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 bonds. 4b. The composition of claim 1b or 2b, wherein the insoluble alpha-glucan particles have a crystallinity of at least about 0.65. 5b. The composition of claim 4b, wherein the insoluble alpha-glucan particles have a crystallinity of at least about 0.7. 6b. A composition of claim 1b, 2b, 3b, 4b, or 5b, wherein the weight-average degree of polymerization (DPw) of the insoluble alpha-glucan is at least 15. 7b. The composition of claim 6b, wherein the DPw of the insoluble alpha-glucan is at least about 35 or 40, or about 35 or 40 to about 100. 8b. The composition of claim 6a, wherein the DPw of the insoluble alpha-glucan is about 35 or 40 to about 60. 9b. The composition of claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, or 8b, which is an aqueous composition (e.g., a dispersion, an emulsion). 10b. The composition of claim 9b, wherein the aqueous composition is a dispersion. 11b. The composition of claim 10b, wherein insoluble alpha-glucan particles are dispersed through at least about 90% of the volume of the dispersion. 12b. The aqueous composition of claim 9b, 10b, or 11b, wherein the aqueous composition has a pH of about 0.0 to about 5.0. 13b. The aqueous composition of claim 9b, 10b, or 11b, wherein the aqueous composition has a pH of about 0.0 to about 1.0 or about 0.0 to about 2.0. 14b. The aqueous composition of claim 9b, 10b, or 11b, wherein the aqueous composition has a pH of about 2.0 to about 4.0, and optionally this pH range provides the composition with an antimicrobial effect (for example, killing or inhibiting the growth / proliferation of microorganisms such as bacteria, yeast, or algae). 15b. The composition of claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, 8b, 9b, 10b, 11b, 12b, 13b or 14b, wherein the temperature of the composition is up to about 125°C. 16b. A composition of claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, 8b, 9b, 10b, 11b, 12b, 13b, 14b or 15b, which is a household care product, a personal care product, an industrial product, an ingestible product (e.g., food), or a pharmaceutical product. 17b. A composition according to claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, 8b, 9b, 10b, 11b, 12b, 13b, 14b, 15b or 16b, wherein (a) a latex composition such as a paint or adhesive; (b) a composition containing a pigment such as a paint or sunscreen; (c) a film or coating such as an edible film or coating; (d) a detergent composition; (e) a composite material comprising at least one polymer in addition to insoluble alpha-glucan particles, wherein the additional polymer is optionally polyurethane, rubber or a thermoplastic polymer; or (f) a capsule material for encapsulating a composition containing a compound, wherein the capsule material optionally allows for controlled release of the compound. 18b. A composition according to claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, 8b, 9b, 10b, 11b, 12b, 13b, 14b, 15b, 16b or 17b, further comprising at least one additive that modifies the mechanical properties of the composition, optionally the additive being selected from crosslinking agents, plasticizers, conditioning agents, dispersants or wetting agents, and optionally the composition being a film or a coating. 19. The composition of claim 1b, 2b, 3b, 4b, 5b, 6b, 7b, 8b, 9b, 10b, 11b, 12b, 13b, 14b, 15b, 16b, 17b or 18b, comprising at least two different phases, wherein the insoluble alpha-glucan particles are located at the interface of the two different phases. 20b. A method for producing insoluble alpha-glucan particles (as described in any of Embodiments 1b to 8b, for example), comprising: (a) providing an insoluble alpha-glucan produced in an enzymatic reaction comprising at least water, sucrose, and a glucosyltransferase enzyme for synthesizing insoluble alpha-glucan, wherein the soluble alpha-glucan has a weight-average degree of polymerization (DPw) of at least about 200, and at least 50% of the glycosidic bonds of the insoluble alpha-glucan are alpha-1,3 glycosidic bonds; (b) hydrolyzing the insoluble alpha-glucan to insoluble alpha-glucan particles having a maximum DPw of about 100, the hydrolysis being carried out under aqueous conditions at a pH of 2.0 or less; and (c) optionally isolating the insoluble alpha-glucan particles produced in step (b). [Examples]

[0204] The following embodiments further illustrate the present disclosure. These embodiments illustrate specific aspects of the present invention, but it should be understood that they are provided solely for illustrative purposes. From the prior discussion and these embodiments, those skilled in the art will be able to identify the essential features of the disclosed embodiments and make various modifications and alterations to adapt the disclosed embodiments to various uses and conditions without departing from the spirit and scope thereof.

[0205] Example 1 Production of highly crystalline, insoluble alpha-glucan This example describes the preparation of crystalline alpha-glucan in the form of an insoluble plate. In particular, an insoluble alpha-1,3-glucan plate was prepared by hydrolyzing enzymatically synthesized alpha-1,3-glucan.

[0206] The insoluble alpha-1,3-glucan used in this embodiment was first prepared by enzymatic synthesis in a manner similar to that described in U.S. Patent Application Publication No. 2018 / 0340199 and U.S. Patent Application Publication No. 2019 / 0078063 (both of which are incorporated herein by reference). Generally, a glucan synthesis reaction was carried out comprising water, sucrose, buffer, filtrate from an earlier glucan synthesis reaction (e.g., containing gluco-oligosaccharide byproducts from an earlier glucan synthesis reaction), and amino acid denaturation, and a high-product-yielding glucosyltransferase enzyme. After this reaction, the alpha-1,3-glucan product (insoluble, about 100% alpha-1,3 bonds, about 800 DPw) was filtered and washed to remove most of the fructose and other residual soluble sugars (e.g., glucose, sucrose, leucrose, DP2-DP8 gluco-oligosaccharides). Next, the washed product sample was collected as a wet cake (not dried) with a solid content of approximately 20–40% by weight, or dried to a powder with a solid content of approximately 88–95% by weight using a rotary dryer.

[0207] Next, both undried and dried insoluble alpha-1,3-glucan samples were subjected to hydrochloric acid hydrolysis at 80°C and approximately 0 pH to produce insoluble alpha-1,3-glucan with reduced molecular weight. Each hydrolysis reaction initially contained 8% by weight of alpha-1,3-glucan. To hydrolyze alpha-1,3-glucan to a lower molecular weight but insoluble form, the procedure disclosed in U.S. Patent Application Publication No. 2013 / 0244287 (incorporated herein by reference), which describes the hydrolysis of insoluble alpha-1,3-glucan with mineral acids to soluble alpha-1,3-glucan, can be applied. The hydrolysis reaction was allowed to proceed for 1 hour, 8 hours, 1 day, or 3 days before neutralization. Each hydrolyzed insoluble alpha-1,3-glucan product was then analyzed in terms of molecular weight. Figure 1 shows that after one day of hydrolysis of undried or dried insoluble alpha-1,3-glucan, insoluble alpha-1,3-glucan with a weight-average degree of polymerization (DPw) of approximately 40–60 was produced. In particular, this molecular weight was stable and remained similar throughout the hydrolysis period under very low pH conditions (Figure 1). In another hydrolysis, insoluble alpha-1,3-glucan with a DPw of approximately 39 was produced (data not shown).

[0208] The crystallinity (or crystallinity index [CI]) of alpha-1,3-glucan samples was measured by wide-angle X-ray dispersion (WAXS) as follows: Glucan powder samples were dried in a vacuum oven set to 60°C for a minimum of 2 hours or overnight (sometimes over the weekend). Immediately before starting the diffraction scan, each sample was removed from the oven and transferred to a stainless steel holder with a well measuring 1.5 cm wide × 4 cm long × 4 mm deep. A glass plate was clipped to the top of the holder, and the well was opened on the side to allow the powder to be poured in from the side. Throughout the filling process, the powder was filled several times by repeatedly striking the opposite side of the holder against the table. Finally, the holder was returned to its correct orientation, the glass plate was removed, and the holder was loaded into the diffractometer. The time from opening the oven to starting the scan was less than 5 minutes. A reflection-mode X'PERT MRD powder diffractometer (PANalytical BV, The Netherlands) was used to measure the X-ray diffraction pattern of each powder sample. The X-ray source was a Cu X-ray tube source equipped with an optical focusing mirror and a 1 / 16° narrow slit. The X-rays were detected using a 1-D detector and a scattering prevention slit set to 1 / 8°. Data were collected in the 2θ range of 4–60° at a step of 0.1°. The scanning took approximately 46 minutes in total. Subsequently, the obtained X-ray patterns were analyzed by subtracting a linear baseline from 7.2–30.5°, subtracting the XRD pattern of a known amorphous alpha-1,3-glucan sample scaled to fit the data being analyzed, and then fitting the remaining crystalline peaks in that range with a series of Gaussian curves corresponding to the reflections of known dehydrated alpha-1,3-glucan crystals. The crystallinity index was then obtained by dividing the area corresponding to the crystalline peaks by the total area under the curve after subtracting the baseline.

[0209] The crystallinity of the alpha-1,3-glucan samples prepared above by hydrolysis was compared with that of enzymatically polymerized alpha-1,3-glucan that was not hydrolyzed. Figure 2 shows that hydrolyzed alpha-1,3-glucan has substantially higher crystallinity (greater than 0.65) compared with unhydrolyzed alpha-1,3-glucan. In particular, hydrolyzed alpha-1,3-glucan with a DPw of 50 (prepared by acid hydrolysis of a wet cake as described above at 40°C for 48 hours) had a crystallinity of approximately 0.76 (Figure 2, left square). A sample of hydrolyzed alpha-1,3-glucan with a DPw of 94 (prepared by acid hydrolysis of a wet cake as described above at 40°C for 1 hour) had a crystallinity of approximately 0.69 (Figure 2, left square). However, samples of enzymatically produced, unhydrolyzed alpha-1,3-glucan (approximately 100% alpha-1,3 linkage) with a DPw in the range of approximately 230 to 830 exhibited low crystallinity (Figure 2, black circles) (the molecular weight of enzymatically produced alpha-1,3-glucan can be modulated to be within the range of DPw 230 to 830 using, for example, the technique described in U.S. Patent Application Publication No. 2015 / 0064748 (incorporated herein by reference)).

[0210] Using electron microscopy, the microstructure of hydrolyzed alpha-1,3-glucan (DPw50, 0.76 CI, 1.2 PDI) was compared with that of unhydrolyzed alpha-1,3-glucan (DPw approximately 800) (as prepared above) (Figures 3A-D). Glucan samples were imaged by dry cast electron microscopy using phosphotungstate as a contrast agent, as described below. Slurries of alpha-1,3-glucan with DPw50 and DPw approximately 800 were purified by multiple centrifugations and redispersion in DI water. The final purified glucan samples were diluted 100-fold and then sonicated for 3 minutes. After sonication, the supernatant was isolated from each preparation, and dry cast transmission electron microscopy (TEM) samples were prepared on a copper mesh TEM grid. Phosphate tungstic acid was then used for negative contrast staining, followed by TEM imaging. The resulting TEM images were typically from the edges of larger, thicker samples deposited on the TEM grid. Hydrolyzed alpha-1,3-glucan (DPw 50) exhibited a two-dimensional structure (material greater than approximately 90 wt% that did not aggregate was in plate form) (Figures 3B and 3D), whereas unhydrolyzed alpha-1,3-glucan (DPw approximately 800) exhibited a larger three-dimensional fibrillary structure (Figures 3A and 3C). TEM images of unhydrolyzed alpha-1,3-glucan (approximately 100% alpha-1,3 linkage) that was enzymatically produced and had a DPw of approximately 260 showed a microstructure very similar to that of unhydrolyzed alpha-1,3-glucan (DPw approximately 800) (data not shown).

[0211] Particle size measurements by light scattering analysis of aqueous dispersions showed that hydrolyzed alpha-1,3-glucan (DPw50) had a particle size distribution in which approximately 90% by weight of all particles had a diameter of less than 1 micron (D50 values ​​ranged from approximately 0.15 to 0.2 microns, but could be in the range of approximately 0.1 to 1.0 microns), while unhydrolyzed alpha-1,3-glucan (DPw approximately 800) had a particle size distribution in which >80% by weight of all particles had a diameter of more than 10 microns (D50 values ​​ranged from approximately 10 to 20 microns, but could be in the range of approximately 5 to 50 microns) (Figure 4).

[0212] Example 2 Aqueous dispersions of highly crystalline, insoluble alpha-glucan are stable through changes in pH. This example illustrates the effect of reducing pH on the viscosity of aqueous dispersions of highly crystalline insoluble alpha-glucan or amorphous alpha-glucan. In particular, the dispersion of insoluble alpha-1,3-glucan (DPw 50, 0.76 CI) maintained a stable viscosity profile under low pH conditions, while the dispersion of insoluble alpha-1,3-glucan (DPw approximately 800) showed a change in viscosity under the same conditions.

[0213] An aqueous dispersion (5% by weight, room temperature) of insoluble alpha-1,3-glucan (DPw 50, 0.76 CI, prepared in Example 1) or insoluble alpha-1,3-glucan (DPw approximately 800, prepared in Example 1) was prepared and adjusted to pH 2.0 or 6.4. The aqueous dispersion was then analyzed for viscosity (1-1000 s). -1(Using a Brookfield viscometer at the shear rate) (Figures 5A-B). At pH 6.4, the alpha-1,3-glucan dispersion with DPw 50 showed a viscosity profile approximately two orders of magnitude higher than that of the alpha-1,3-glucan dispersion with DPw approximately 800 (Figure 5A). It should also be noted that the alpha-1,3-glucan dispersion with DPw 50 at pH 2.0 showed no change in viscosity profile compared to the neutral condition at pH 6.4 (Figure 5B). Such an unchanging viscosity profile is unique, as other polysaccharides such as nanocellulose and microcrystalline cellulose show a significant decrease in viscosity under low pH conditions (see U.S. Patent No. 2,978446, incorporated herein by reference).

[0214] The unique high viscosity and pH stability of low-concentration (5 wt%, above) insoluble alpha-1,3-glucan (DPw50, 0.76 CI) enable good compatibility when mixed in low-pH latex dispersions. Figure 6 specifically compares aqueous preparations initially prepared as dispersions (room temperature, pH 4.0) containing 4 wt% alpha-1,3-glucan (DPw50 or DPw approximately 800 from above) and 14 wt% vinyl acetate / ethylene (VAE) latex. The VAE dispersion with DPw50 alpha-1,3-glucan remained stable for at least 3 weeks (the dispersion was discarded after this period) and is considered stable for at least 6–12 months, while DPw approximately 800 alpha-1,3-glucan precipitated from the VAE dispersion in less than 1 hour (Figure 6). Typically, latex dispersions are pH-stabilized at either pH 3–4 or pH 8–9, but the low pH conditions of pH 3–4 present challenges in using polysaccharides in latex dispersions under such pH-stabilized conditions. Alpha-1,3-glucan with a DPw of approximately 800 has been shown to be somewhat stable in such low-pH dispersions at higher concentrations (data not shown), but its instability at 4 wt% as shown herein suggests that its use at low concentrations (e.g., >5 wt%) is problematic. Therefore, it is noteworthy that insoluble alpha-1,3-glucan (DPw 50) was stable and dispersible under these conditions.

[0215] Example 3 Highly crystalline, insoluble alpha-glucan can be used as a pigment extender in paint compositions. This example describes the use of highly crystalline, insoluble alpha-glucan as a pigment extender in a paint composition. In particular, insoluble alpha-1,3-glucan (DPw50, 0.76 CI) was used to replace titanium dioxide (TiO2) pigment in the paint, enhancing the opacity function of this pigment. Such enhancement is associated with the ability to reduce the amount of TiO2 used in the paint.

[0216] TiO2 is the most widely used white pigment in paints due to its high refractive index. The problem with using TiO2 as a pigment is the inherent colloidal instability of TiO2 particles. To address this problem, TiO2 particles are usually coated with SiO2. However, even with an SiO2-coated structure, if the TiO2 particles are not properly spaced (the ideal spacing is about 200 nm), the effectiveness of TiO2 particles as a pigment decreases.

[0217] TiO2 particle-spacing additives are called TiO2 extenders. In this example, it was found that insoluble alpha-1,3-glucan (DPw50, 0.76 CI) can be used as an efficient TiO2 extender in paints, as described below. White paint formulations were generally prepared as follows. The control paint formulation (without alpha-1,3-glucan) contained TiO2 pigment at a pigment concentration of 65 (PVC), while the paint formulations in this experiment contained insoluble alpha-1,3-glucan (either the DPw50 or DPw approximately 800 sample mentioned above) by substituting a specific portion of the TiO2 pigment component. Such substitutions were based on a ratio of TiO2 to alpha-1,3-glucan of 1.0 to 0.6 (based on PVC in the formulation). The paint, formulated using 3 milbars, was applied and dried overnight at approximately 70°C and 50% humidity. The L* (whiteness) and opacity (Y) levels of the dried paint were then measured as described in International Publication No. 2019046123 (incorporated herein by reference) (Table 1).

[0218] [Table 1]

[0219] In particular, as shown in Table 1, replacing TiO2 with alpha-1,3-glucan from DPw50 resulted in a continuous increase in whiteness (L*) and opacity.

[0220] Example 4 Highly crystalline, insoluble alpha-glucans possess unique optical properties. This example describes the preparation of optically transparent products using crystalline insoluble alpha-glucan. In particular, materials containing insoluble alpha-1,3-glucan (DPw 50, 0.76 CI) showed high optical transparency, while materials containing insoluble alpha-1,3-glucan (DPw approximately 800) showed much lower optical transparency.

[0221] Wet cakes of alpha-1,3-glucan (above) with DPw50 or DPw approximately 800 were prepared to contain approximately 28.3% by weight or 33.7% by weight of glucan, respectively. Single layers of either of these wet cakes in paste form, approximately 1–5 mm thick, were then spread onto aluminum pans and photographed before drying. In particular, the alpha-1,3-glucan composition with DPw50 was optically transparent at a visual level, while the alpha-1,3-glucan composition with DPw approximately 800 lacked such transparency (Figure 7). Specifically, black "X" marks were clearly visible under the alpha-1,3-glucan material with DPw50, but were not visible under the hazy alpha-1,3-glucan material with DPw approximately 800 (Figure 7).

[0222] Example 5 Aqueous dispersions of highly crystalline, insoluble alpha-glucan are stable. This example illustrates the effect of drying (before glucan dispersion) on the viscosity of aqueous dispersions of highly crystalline insoluble alpha-glucan or amorphous alpha-glucan. In particular, the dispersion of dried insoluble alpha-1,3-glucan (DPw50, 0.76 CI) showed a viscosity profile similar to that of the undried material, while the dispersion of dried insoluble alpha-1,3-glucan (DPw approximately 800) showed significantly reduced viscosity formation compared to its undried form. The viscosity-forming ability of alpha-1,3-glucan with DPw50 represents another advantage of this material, even in its dried form.

[0223] Wet cakes of alpha-1,3-glucan (described above) with a DPw of 50 or approximately 800 were prepared to contain approximately 40% by weight of glucan. Each of these samples was then dried at 40–110°C to obtain a powder with approximately 88–95% by weight of solids. Each of the wet cake and dried powder samples was individually mixed with deionized water (room temperature, neutral pH) by shaking by hand (without using an automated device) at a solid content of 10% by weight. Each of these preparations was then processed at room temperature for 10 minutes at 10,000 rpm (revolutions per minute) using a handheld rotor stator (IKA T-25). The resulting preparations (see below), representing all but one of the dispersions, were then evaluated for viscosity as described in Example 2.

[0224] As shown in Figure 8, the aqueous preparation of alpha-1,3-glucan with a dried DPw of approximately 800 had a substantially lower viscosity level than the preparation in its undried form, with a viscosity of less than 0.15% of the viscosity of the undried material. This result was consistent with the observation that the dispersion formed by the latter preparation was stable, while the former preparation formed almost no dispersion (data not shown). In particular, the dispersion of alpha-1,3-glucan with a dried DPw of 50 had a viscosity level comparable to the viscosity of the undried form in the dispersion (in the range of approximately 20-50%) (Figure 8). Furthermore, the dispersions of alpha-1,3-glucan with either dried or undried DPw of 50 were stable (data not shown).

[0225] Example 6 Emulsion stabilization by highly crystalline, insoluble alpha-glucan This example demonstrates that highly crystalline, insoluble alpha-glucans can stabilize emulsions. In particular, insoluble alpha-1,3-glucan (DPw50, 0.76 CI) demonstrated a stabilizing effect on emulsions with a narrow droplet size distribution.

[0226] Alpha-1,3-glucan with a DPw of 50 (0.76 CI) was added to a 50:50 mixture of dodecane and water at a concentration of 0.5 or 2.0% by weight. Alpha-1,3-glucan with a DPw of approximately 800 (undried, 40% by weight wet cake) and alpha-1,3-glucan fibrils (prepared according to U.S. Patent Application Publication No. 2018 / 0119357, incorporated herein by reference) were similarly added to the dodecane:water mixture. Each preparation was then homogenized for 2 minutes at 35,000 rpm using a rotor-stator homogenizer (Pro Scientific Pro 250). The resulting emulsions containing dodecane droplets dispersed in water were analyzed for droplet size and stability. Droplet size was measured using a confocal laser scanning microscope in which the dodecane phase was colored with a contrast dye (perylene, 0.01 mg / mL). The rheology of each emulsion was measured using a stress-controlled rotational rheometer (Anton Paar MCR-302) with a parallel plate configuration and a 1 mm spacing.

[0227] Droplet diameter measurements were performed directly on each emulsion to calculate the average emulsion droplet diameter. Rheological measurements of the emulsions were used to calculate their average storage modulus (Avg. G') in the viscoelastic region. These analytical results are shown in Table 2 below. The effect of emulsion stabilization (i.e., Avg. G', emulsion droplet diameter) differed for each of the alpha-1,3-glucan materials tested. The alpha-1,3-glucan sample with DPw 50 was unique compared to the DPw approximately 800 and fibrillary alpha-1,3-glucan samples because it stabilized the emulsion droplet diameter (small droplet diameter with a low standard deviation, i.e., uniform small droplets) and increased the modulus (an increase in Avg. G' indicates an increase in elasticity). Therefore, the highly crystalline, insoluble alpha-1,3-glucan of this disclosure (e.g., DPw50, 0.76 CI) can be used alone as an emulsion stabilizer or in combination with other stabilizers (e.g., alpha-1,3-glucan fibrils).

[0228] [Table 2]

[0229] Example 7 Encapsulation with highly crystalline, insoluble alpha-glucan In this embodiment, a dry emulsion is formed using highly crystalline insoluble alpha-glucan. The component particles of these emulsions contain a stabilized material core encapsulated by an insoluble alpha-glucan shell. In particular, insoluble alpha-1,3-glucan (DPw50, 0.76 CI) was used to encapsulate oil (shea nut butter), thereby forming particles with a hydrophobic core.

[0230] A mixture of DPw50 (0.76 CI) alpha-1,3-glucan, water, and shea nut butter was prepared in a ratio of 2 (glucan):20 (water):11 (shea nut butter). To dissolve the shea nut butter, the mixture was heated to 60°C under vibration. To form a liquid emulsion of the mixture, it was homogenized for 5 minutes at 20 krpm using a rotor-stator homogenizer (Ultra-Turrax T25, IKA). The stability of the emulsion was visually confirmed.

[0231] The emulsion was freeze-dried or spray-dried to produce a dry powder form of the emulsion. For freeze-drying, the emulsion was rapidly cooled using dry ice and dried for 48 hours under vacuum at -50°C.

[0232] For spray drying, the emulsion was spray-dried using a spray dryer (Yamato Pulvis GB22) equipped with an external peristaltic pump (Cole-Palmer Masterflex L / S) with a #14 silicone tube (Precision Pump). Atomization was performed using a two-fluid nozzle, with air used as the spray gas at 7 psi. The drying airflow velocity was 0.68 m 3The temperature was per minute, the dry inlet temperature was 120°C, and the outlet temperature was 50°C.

[0233] Each powder, prepared by freeze-drying or spray-drying, was imaged at 5000x magnification using scanning electron microscopy (SEM). The SEM was performed using an FEI QUANTA 650 unit operated at an acceleration voltage of 0.8–1 mbar and 10 kV. Each dried powder emulsion was observed to contain particles with a shea nut butter core and an alpha-1,3-glucan protective shell (see, for example, Figure 9).

[0234] Example 8 Edible coating containing highly crystalline, insoluble alpha-glucan This example demonstrates that highly crystalline insoluble alpha-glucans can be used in edible coatings on foods such as fruits and vegetables. Such edible coatings can be used, for example, to increase the shelf life of food. In particular, insoluble alpha-1,3-glucan (DPw50, 0.76 CI) was used in an edible coating on avocados. As determined by two different analyses, the coating with insoluble glucan inhibited fruit ripening compared to uncoated samples.

[0235] Unripe avocados were immersion-coated with a dispersion of 6-9% by weight of insoluble alpha-1,3-glucan (DPw50, 0.76CI) (in water) and stored for one week at 85% relative humidity (RH) at 5 or 20°C. The ripening of the coated avocado samples was compared to that of uncoated avocado samples stored under the same conditions. Ripeness was classified using the following five-stage ready-to-eat (RTE) classification: Stage 1: Insufficient RTE, too hard (this stage generally characterizes unripe avocado samples at the start of these analyses). Stage 2: Sufficient RTE, but somewhat stiff. Stage 3: Sufficient RTE. Stage 4: Sufficient RTE, but somewhat soft. Stage 5: Insufficient RTE, too soft.

[0236] These analytical results are as follows, demonstrating that coating with the insoluble alpha-1,3-glucan specified herein can prevent fruit ripening: Uncoated sample, 5°C: RTE step 1-2. Uncoated sample, 20°C: RTE step 3-4. Coated sample, 20°C: RTE step 1.

[0237] Furthermore, (overlapping) the release of ethylene from avocado samples at 20°C was tracked over time by gas chromatography. Ethylene production was tracked (parts per million [ppm]) for 4 days. As shown in Table 3, coated avocados showed significantly lower ethylene production. This result is consistent with the above findings that fruit ripening can be prevented by coating with the insoluble alpha-1,3-glucan specified herein.

[0238] [Table 3]

[0239] Example 8 Barrier coating containing highly crystalline, insoluble alpha-glucan This embodiment demonstrates the use of highly crystalline, insoluble alpha-glucans in product barrier coatings. These barriers can provide protection against hydrophobic substances such as oils. In particular, when paper was coated with an aqueous preparation containing insoluble alpha-1,3-glucan (DPw50, 0.76 CI) and other components, these paper coatings exhibited resistance to oil absorption.

[0240] Insoluble alpha-1,3-glucan (DPw50, 0.76 CI) was dispersed in two different ratios: 8 or 5 parts WSCG, PVOH, or starch to 2 or 5 parts insoluble alpha-1,3-glucan (based on the weight percentage of each component in the final preparation). Each preparation was then coated onto a paper substrate using an automated film applicator (ZAA2600 ZEHNTNER, RDS 3 rods). As a control, a preparation using 10% by weight WSCG, PVOH, or starch, but without the addition of insoluble alpha-1,3-glucan, was coated onto paper. The coated paper was dried to a depth of 25 cm. 2 Cut into sheets and use a bump tester (internal area 10 cm²). 2 Analysis was performed using ). Specifically, coated paper was exposed to either 10 mL of water or castor oil for 60 seconds. At the 45-second mark, the content was measured, and the paper was carefully removed from the clamp. Then, to remove excess water or oil, each paper sample (its weight was measured in "m") at the 45-second mark was measured. dry The paper (provided as "m") was wiped and rolled using a 10kg roller. The final weight of the paper ("m") was determined. exposed The Cobb value (g / m²) of each sample was measured using the following formula. 2 ) was calculated.

number

[0241] The Cobb value (Cobb index value) provides a standard for the absorption of applied liquids by paper, with higher values ​​indicating greater absorption. The following Cobb index value range was used to characterize the degree of water or oil absorption by paper in the above tests.

[0242] [Table 4]

[0243] The cob index values measured for the above samples are listed in Table 4 below.

[0244]

Table 5

[0245] Based on the data in Table 4, it is clear that the addition of the insoluble alpha-‌1,3-‌glucan of the present specification can enhance the barrier properties of PVOH and starch against hydrophobic substances, particularly at a ratio of 2 parts glucan to 8 parts of this barrier material. The above results similarly characterize what is observed when paperboard or flex paper is used as the paper substrate for coating (data not shown).

[0246] Example 9 Reinforcement of Rubber Composites Using Highly Crystalline Insoluble Alpha-‌Glucan This example shows that the insoluble alpha-‌glucan of the present specification provides reinforcement to the physical and mechanical properties of rubber composites. In particular, a rubber composition containing insoluble alpha-‌1,3-‌glucan (DPw50, 0.76CI) was prepared and analyzed. Based on this analysis, it is considered that the insoluble alpha-‌glucan of the present disclosure can be used to reinforce rubber-‌containing products such as tires.

[0247] To incorporate insoluble alpha-‌1,3-‌glucan (DPw50, 0.76CI) into the rubber composite, a masterbatch of this insoluble alpha-‌glucan (30 wt% loading) in natural rubber (NR) was prepared. An aqueous dispersion of insoluble alpha-‌glucan particles (7 wt%) and NR latex (60 wt%) were mixed together to form a slurry and coagulated using formic acid (5 vol%). The coagulum was divided into smaller parts, dried, and milled. For rubber compounding, the dried coagulum (i.e., masterbatch) (<3% moisture) was used.

[0248] The masterbatches prepared above were mixed with rubber additives in an internal mixer in two paths according to the formulations shown in Table 5 below. In the first path, the mixer was heated to 120°C and a masterbatch containing all additives except sulfur and CBS was added. During mixing, the temperature was raised to 150°C and held at 150°C for 2 minutes. As a comparative example, an NR masterbatch containing silica or carbon black was added in place of insoluble alpha-glucan in the first path. In the second path, the mixer was heated to 80°C and the mixed rubber from the first path, sulfur, and CBS were added. Each rubber preparation was mixed until the temperature reached 95°C. After each rubber preparation cooled, it was milled in a two-roll mill, then compression-molded to cure into test specimens, which were then characterized.

[0249] [Table 6]

[0250] Natural rubber composites containing insoluble alpha-1,3-glucan as a filler and comparative natural rubber composites containing conventional fillers (carbon black or silica) were tested for their physical and mechanical properties. Natural rubber composites without fillers were also tested in the same manner. The results of these analyses are summarized in Table 6 below.

[0251] [Table 7]

[0252] From Table 6, we can conclude the following:

[0253] • Insoluble alpha-1,3-glucan NR composites have a lower density compared to existing fillers. Therefore, for example, the insoluble alpha-1,3-glucan disclosed herein is suitable for weight reduction purposes.

[0254] As a filler, insoluble alpha-1,3-glucan demonstrates an overall improvement in physical properties (tensile strength, elongation, and modulus of elasticity) compared to high-performance silica (Ultrasil GR 7000) fillers, without requiring a silane coupling agent (Si69).

[0255] The insoluble alpha-1,3-glucan NR composite material has the lowest tandelta at 60°C. Therefore, compared to using silica or carbon black instead, tires having the insoluble alpha-1,3-glucan disclosed herein have good rolling resistance.

[0256] • The insoluble alpha-1,3-glucan mixture has a curing time comparable to that of N234 carbon black, but with a much lower M L It has good processing properties.

[0257] Example 10 Reinforcement of polyurethane films with highly crystalline, insoluble alpha-glucan This example demonstrates that the insoluble alpha-glucan described herein can enhance the mechanical and tensile properties of polyurethane compositions. In particular, polyurethane films containing insoluble alpha-1,3-glucan (DPw50, 0.76 CI) were prepared and analyzed.

[0258] Insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles were mixed with propanediol (PDO)-sebacate polyol-based polyurethane dispersions (PUDs) (Troy Polymers Inc.) at various loading levels to produce various one-component polyurethane dispersions (1K-PUDs). The detailed formulations before PUD are shown in Table 7 below.

[0259] [Table 8]

[0260] Samples of PUD were loaded with different amounts of insoluble alpha-1,3-glucan particles (provided as a 10 wt% dispersion in water), providing preparations having 1-50 wt% insoluble alpha-glucan (based on total solids). All of these PUD preparations were stable without showing any signs of phase separation. Next, each formulation was blade coated onto polypropylene sheets using a drawdown wire rod #40 to form films. The contents of these formulations (precoatings) and the insoluble alpha-glucan content of the dried films are listed in Table 8 below.

[0261]

Table 9

[0262] Next, an INSTRON instrument was used to measure the tensile properties of each film. The results of this analysis are shown in Table 9 below.

[0263]

Table 10

[0264] After hydrolysis aging (50 °C, 95% RH, 3 days), the films were further analyzed as shown in Table 10 below.

[0265]

Table 11

[0266] The addition of the insoluble alpha-1,3-glucan disclosed herein into films prepared from polyurethane dispersions resulted in a positive improvement in the mechanical properties of the films. These improvements occurred regardless of the presence or absence of hydrolysis aging of the films (Tables 9 and 10).

[0267] The films were also tested for hardness (ASTM D3363-20, Standard Test Method for Film Hardness by Pencil Test, ASTM International, 2020) and adhesion (ASTM D3359-17, Standard Test Methods for Rating Adhesion by Tape Test, ASTM International, 2017) (both ASTM tests are incorporated herein by reference). Films containing 10% by weight and 30% by weight of insoluble alpha-1,3-glucan showed improved hardness from H to 2H (ASTM D3363) and improved adhesion from 4A to 5A (ASTM D3359).

[0268] Example 11 Melt-processable polyurethane composition containing highly crystalline insoluble alpha-glucan This example demonstrates that the water-free masterbatch containing the insoluble alpha-glucan and polyurethane specified herein is melt-processable.

[0269] A dispersion of insoluble alpha-1,3-glucan particles (DPw50, 0.76 CI) (8 wt% in water) was blended with a polyurethane dispersion (the same formulation as listed in Table 7 of Example 10) in a 50 / 50 ratio using an overhead mixer at 200 rpm for 5 minutes. The blended formulation (10 wt% solids) was dried in a vacuum oven at 80°C for 48 hours to completely remove water. This drying yielded a hard, whitish, brittle masterbatch preparation that could be molded by the application of heat. For example, a transparent film was prepared by heat-compressing the masterbatch-dried powder at 105°C and 20,000 psi for 5 minutes. The high optical transparency (transparency) of the film indicated that the insoluble alpha-1,3-glucan component was well dispersed in the polyurethane matrix and that the glucan had a unique particle size and morphology that did not cause opacity.

[0270] Example 12 Gas barrier coating containing highly crystalline, insoluble alpha-glucan This embodiment demonstrates that highly crystalline, insoluble alpha-glucan can be used in barrier coatings to protect products from gas elements. In particular, a barrier formed from an aqueous preparation containing insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles reduced the oxygen permeation rate.

[0271] Films containing insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles, butenediol vinyl alcohol copolymer (BVOH), and glycerol were cast. For this purpose, aqueous solutions of BVOH and glycerol were prepared, divided into aliquots, and then insoluble alpha-1,3-glucan particles were mixed into each aliquot at different concentrations. One aliquot contained no insoluble glucan (blank / control). Individual films were then cast using each of these preparations and subsequently dried. The blank / control film contained approximately 90% by weight of BVOH and approximately 10% by weight of glycerol, while the other films contained increased amounts of insoluble glucan (5, 10, or 20% by weight). Each film was then tested for its oxygen permeability (OTR) at 23°C with 100% O2 at 35% or 50% relative humidity (RH). The results of this analysis are shown in Table 11 below.

[0272] It is known that BVOH has relatively good OTR properties and that this quality changes with the effect of RH. At low RH, BVOH has good oxygen barrier properties (i.e., low OTR), but this advantage decreases at higher RH (i.e., OTR increases). The data in Table 11 show that the inclusion of the insoluble alpha-1,3-glucan disclosed herein in a BVOH-containing film significantly enhances the oxygen barrier capacity of the film under both tested RH conditions. Therefore, the insoluble alpha-1,3-glucan particles disclosed herein can be used to increase the oxygen barrier properties of compositions such as films, while also providing the advantages of increased bio-content and biodegradability.

[0273] [Table 12]

[0274] Example 13 Use of highly crystalline, insoluble alpha-glucan as a binder in nonwoven fabrics This example demonstrates that highly crystalline insoluble alpha-glucan can be used as a binder / reinforcement in nonwoven fabric products, and that this effect can be enhanced when the glucan is crosslinked. In particular, the tensile strength of nonwoven fabrics of two different types of pulp fibers was increased by treatment with crosslinked or uncrosslinked insoluble alpha-1,3-glucan (DPw50, 0.76CI) particles.

[0275] Airlaid nonwoven sheets containing 100% fluff pulp (Georgia-Pacific) were sprayed with a dispersion of crosslinked or uncrosslinked insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles and then dried in a heated oven at 140°C for 5 minutes. Alpha-1,3-glucan particle crosslinking was performed using glyoxal, citrate, or polyamidoamine-epichlorohydrin (PAE). Upon drying, the sheets that received the glucan particles contained 80 wt% pulp and (i) 20 wt% glucan (uncrosslinked particles) or (ii) 16 wt% glucan and 4 wt% crosslinking agent. The dried nonwoven sheets were then analyzed for their dry and wet tensile strength properties using EDANA standard NWSP 110.1.R0 (incorporated herein by reference). The above procedures / analyses were also performed using wet-laid nonwoven sheets of 100% Northun-bleached softwoodcraft (NBSK) pulp (Domtar). The results of this study are shown in Table 12 below.

[0276] [Table 13]

[0277] The data in Table 12 demonstrates that the uncrosslinked and crosslinked insoluble alpha-1,3-glucan particles of this disclosure can reinforce nonwoven materials.

[0278] Example 14 Light dispersion by highly crystalline insoluble alpha-glucan This embodiment discloses that the insoluble alpha-glucan particles of the present disclosure have photodispersive properties and can therefore be used as a photodispersive additive in compositions such as liquids. In particular, a dispersion of insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles in water has been shown to scatter light.

[0279] Dispersions of insoluble alpha-1,3-glucan (DPw50, 0.76 CI) particles in water at different concentrations (0.008, 0.08, 0.8, 8.0 wt%) were measured for scattering of 500 nm wavelength light. The amount of scattered light was measured in arbitrary units (au) using a CARY 100 UV-VIS spectrometer. The data listed in Table 13 below demonstrate that dispersed alpha-glucan particles can effectively scatter light. Even at a loading level of 0.08 wt%, the dispersed particles showed a significant amount of light scattering. Furthermore, it was found that the dispersed insoluble alpha-1,3-glucan did not absorb any light in the visible spectrum (i.e., the particles formed a white dispersion).

[0280] [Table 14]

Claims

1. A composition comprising water-insoluble alpha-glucan particles having a crystallinity of at least 0.7, wherein the water-insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of 15 to 100, and at least 50% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 glycosidic bonds. At least 80% by weight of the water-insoluble alpha-glucan particles are in the form of plates. The composition is a household care product selected from laundry detergent, fabric softener, hard surface cleaner, automatic dishwasher detergent, or hand dishwashing detergent.

2. A composition comprising water-insoluble alpha-glucan particles having a crystallinity of at least 0.7, wherein the water-insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of 15 to 100, and at least 50% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 glycosidic bonds. At least 80% by weight of the water-insoluble alpha-glucan particles are in the form of plates. The composition is a personal care product selected from lotions, creams, pastes, mineral oils, ointments, pomades, or gels.

3. A composition comprising water-insoluble alpha-glucan particles having a crystallinity of at least 0.7, wherein the water-insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of 15 to 100, and at least 50% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 glycosidic bonds. At least 80% by weight of the water-insoluble alpha-glucan particles are in the form of plates. Drywall tape bonding compounds, mortar, grout, cement plaster, spray plaster, cement stucco, adhesives, pastes, wall / ceiling binders, insecticides, herbicides or fertilizer spray adhesives or suspension / dispersion aids, polymer emulsions, latex, gels, paints, protective coatings, sealants, caulking agents, inks, metal cutting The composition is an industrial product selected from a drilling fluid, a film or coating, or an emulsion-based metal cleaning solution.

4. A composition comprising water-insoluble alpha-glucan particles having a crystallinity of at least 0.7, wherein the water-insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of 15 to 100, and at least 50% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 glycosidic bonds. At least 80% by weight of the water-insoluble alpha-glucan particles are in the form of plates. The composition is an ingestible product selected from food, beverages, animal feed, or animal health or nutrition products.

5. A composition comprising water-insoluble alpha-glucan particles having a crystallinity of at least 0.7, wherein the water-insoluble alpha-glucan has a weight-average degree of polymerization (DPw) of 15 to 100, and at least 50% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 glycosidic bonds. At least 80% by weight of the water-insoluble alpha-glucan particles are in the form of plates. The composition is a pharmaceutical product selected from emulsions, liquids, elixirs, gels, suspensions, creams, or ointments.

6. The composition according to any one of claims 1 to 5, wherein at least 90% of the glycosidic bonds of the water-insoluble alpha-glucan are alpha-1,3 bonds.

7. The composition according to any one of claims 1 to 6, wherein the DPw of the water-insoluble alpha-glucan is 35 to 100.

8. The composition according to any one of claims 1 to 6, wherein the DPw of the water-insoluble alpha-glucan is 35 to 60.

9. The composition according to any one of claims 1 to 8, which is an aqueous composition.

10. The composition according to claim 9, wherein the aqueous composition is a dispersion.

11. The composition according to claim 10, wherein the water-insoluble alpha-glucan particles are dispersed through at least 90% of the volume of the dispersion.

12. The composition according to any one of claims 1 to 9, which is an emulsion.

13. The composition according to any one of claims 1 to 12, wherein at least 70% by weight of the water-insoluble alpha-glucan particles have a diameter of less than 1.0 micron, or 45 to 55% by weight of the water-insoluble alpha-glucan particles have a diameter of less than 0.35 microns.

14. The composition according to any one of claims 1 to 13, wherein the water-insoluble alpha-glucan particles have a crystallinity of at least 0.

75.

15. The composition according to claim 2, wherein the personal care product is a lotion.

16. The composition according to claim 15, which is a sunscreen.

17. (a) Latex composition; (b) Compositions containing pigments; (c) Film or coating; (d) Detergent composition; (e) A composite material comprising at least one polymer in addition to the water-insoluble alpha-glucan particles; or (f) Capsule material for enclosing a composition containing a compound The composition according to any one of claims 1 to 14.

18. The composition according to any one of claims 1 to 14, comprising at least two different phases, wherein the water-insoluble alpha-glucan particles are located at the interface of the two different phases.

19. The composition according to claim 1, wherein the household care product is a laundry detergent.

20. The composition according to claim 1, wherein the household care product is a detergent for automatic dishwashers.

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