Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/73—Polysaccharides
  • A61K8/733—Alginic acid; Salts thereof
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING OR TREATMENT THEREOF
  • A23C9/00—Milk preparations; Milk powder or milk powder preparations
  • A23C9/12—Fermented milk preparations; Treatment using microorganisms or enzymes
  • A23C9/13—Fermented milk preparations; Treatment using microorganisms or enzymes using additives
  • A23C9/137—Thickening substances
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
  • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
  • A01N25/10—Macromolecular compounds
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
  • A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
  • A23G1/30—Cocoa products, e.g. chocolate; Substitutes therefor
  • A23G1/56—Liquid products; Solid products in the form of powders, flakes or granules for making liquid products, e.g. for making chocolate milk, drinks and the products for their preparation, pastes for spreading or milk crumb
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
  • A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
  • A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
  • A23G3/346—Finished or semi-finished products in the form of powders, paste or liquids
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
  • A23L19/09—Mashed or comminuted products, e.g. pulp, purée, sauce, or products made therefrom, e.g. snacks
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
  • A23L2/52—Adding ingredients
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
  • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
  • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
  • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
  • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
  • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
  • A23L29/262—Cellulose; Derivatives thereof, e.g. ethers
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
  • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
  • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
  • A61K47/38—Cellulose; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/73—Polysaccharides
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/73—Polysaccharides
  • A61K8/731—Cellulose; Quaternized cellulose derivatives
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
  • A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
  • A61K9/146—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
  • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
  • C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J3/00—Processes of treating or compounding macromolecular substances
  • C08J3/12—Powdering or granulating
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J3/00—Processes of treating or compounding macromolecular substances
  • C08J3/12—Powdering or granulating
  • C08J3/128—Polymer particles coated by inorganic and non-macromolecular organic compounds
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
  • C08L1/02—Cellulose; Modified cellulose
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
  • C08L1/02—Cellulose; Modified cellulose
  • C08L1/04—Oxycellulose; Hydrocellulose, e.g. microcrystalline cellulose
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
  • C08L5/04—Alginic acid; Derivatives thereof
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
  • C08L5/06—Pectin; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
  • A23G2200/00—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents
  • A23G2200/06—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents containing beet sugar or cane sugar if specifically mentioned or containing other carbohydrates, e.g. starches, gums, alcohol sugar, polysaccharides, dextrin or containing high or low amount of carbohydrate
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
  • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
  • A61K2800/41—Particular ingredients further characterized by their size
  • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
  • A61K2800/59—Mixtures
  • A61K2800/594—Mixtures of polymers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
  • C08J2301/04—Oxycellulose; Hydrocellulose
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
  • C08J2305/04—Alginic acid; Derivatives thereof
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/16—Halogen-containing compounds
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L2205/00—Polymer mixtures characterised by other features
  • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

Definitions

• the present invention relates to microcrystalline cellulose compositions, to a process for their manufacture, and to products containing the same. More particularly the invention relates to particulate microcrystalline cellulose compositions having a mean particle size of less than about 10 microns and comprising closely bound microcrystalline cellulose and at least one hydrocoUoid.
• the compositions are prepared by applying a shear force to a high solids mixture of microcrystalline cellulose and a hydrocoUoid by vigorously kneading the mixture in the presence of an anti-slip agent.
• Microcrystalline cellulose is a white, odorless, tasteless, relatively free flowing, crystalline powder that is virtually free from organic and inorganic contaminants. It is a purified, partially depolymerized cellulose obtained by subjecting alpha cellulose obtained as a pulp from fibrous plant material to hydrolytic degradation typically with mineral acid. It is a highly crystalline particulate cellulose consisting primarily of crystalline aggregates which are obtained by removing amorphous (fibrous cellulose) regions of a cellulosic material. MCC is used in a variety of applications including foods, pharmaceuticals and cosmetics.
• Microcrystalline cellulose may be produced by treating a source of cellulose, preferably alpha cellulose in the form of pulp from fibrous plant materials, with a mineral acid, preferably hydrochloric acid. The acid selectively attacks the less ordered regions of the cellulose polymer chain thereby exposing and freeing the crystalline sites which form crystallite aggregates which constitute the microcrystalline cellulose. These are then separated from the reaction mixture, and washed to remove degraded by-products.
• the resulting wet mass generally containing 40 to 60 percent moisture, is referred to in the art by several names, including hydrolyzed cellulose, hydro lyzed cellulose wetcake, level-off DP cellulose, microcrystalline cellulose wetcake or simply wetcake.
• microcrystalline cellulose When the wetcake is dried and freed of water the resulting product, microcrystalline cellulose, is a white, odorless, tasteless, relatively free- flowing powder, insoluble in water, organic solvents, dilute alkalis and acids.
• a pharmaceutical excipient particularly as a binder, disintegrant, flow aid, and/or filler for preparation of compressed pharmaceutical tablets.
• Microcrystalline cellulose and/or hydrolyzed cellulose wetcake has been modified for other uses, notably for use as a gelling agent for food products, a thickener for food products, a fat substitute and/or non-caloric filler for various food products, as a suspension stabilizer and/or texturizer for food products, and as an emulsion stabilizer and suspending agent in pharmaceutical and cosmetic lotions and creams. Modification for such uses is carried out by subjecting micro-crystalline cellulose or wetcake to intense attrition forces as a result of which the crystallites are substantially subdivided to produce finely divided particles.
• a protective colloid such as sodium carboxy- methylcellulose (CMC), which wholly or partially neutralizes the bonding forces which cause agglomeration or hornification, may be added during attrition or following attrition but before drying. This additive also facilitates re-dispersion of the material following drying.
• CMC carboxy- methylcellulose
• the resulting material is frequently referred to as attrited microcrystalline cellulose or colloidal microcrystalline cellulose.
• Colloidal microcrystalline cellulose is a white odorless, hygroscopic powder. On being dispersed in water, it forms white, opaque thixotropic gels with microcrystalline cellulose particles less than 1 micron in size. It is manufactured and sold by FMC Corporation (FMC) in various grades under the designations, among others, Avicel RC and Avicel CL, which comprise co-processed microcrystalline cellulose and carboxymethylcellulose sodium.
• FMC FMC Corporation
• CMC in a colloidal microcrystalline cellulose by using a combination of additives consisting of a first ingredient which is a carbohydrate sweetner, e.g., sucrose, dextrose, or hydrolyzed cereal solids, and a second ingredient which is a hydrocoUoid, e.g., guar gum, locust bean gum, gum arabic, sodium alginate, propylene glycol alginate, carrageenan, gum karaya, or xanthan gum.
• a carbohydrate sweetner e.g., sucrose, dextrose, or hydrolyzed cereal solids
• a hydrocoUoid e.g., guar gum, locust bean gum, gum arabic, sodium alginate, propylene glycol alginate, carrageenan, gum karaya, or xanthan gum.
• MCC-based stabilizing agent is described by Tuason et al. in US Pat. No. 5,366,742. This agent is prepared by mixing colloidal MCC with sodium alginate in water and then adding a soluble calcium salt to the slurry in an amount which deposits a sodium, calcium alginate complex on the surface of the MCC to provide barrier coating properties. After homogenization, the slurry is spray dried. The resulting stabilizing agent may be redispersed in water by use of high shear methods which appear to break the calcium alginate crosslinks, thus allowing dispersion to occur.
• the flocculated product is claimed to be comprised of spherical particles ranging in size from 0.1 to 100 microns.
• spray dried powder has a particle size range of 5-70 microns. Reconstitution or rehydration of this coprocessed material requires high shear conditions. In compositions having 15 weight % or more of the galactomannan gum, high shear dispersion of the spray-dried material results in fibrous particles. Either the spherical aggregates or the fibrous material is particularly effective in providing fat-like properties to foodstuffs.
• U.S. 6,391,368 discloses a composition comprising attrited colloidal microcrystalline wetcake which is coprocessed with iota carrageenan and dried.
• the composition is prepared by the following process:
• U.S. 6,037,380 discloses a composition comprising microcrystalline cellulose, a relatively water insoluble attriting aid and, optionally a protective colloid.
• the compositions are prepared by the following process: (a) blending together unattrited microcrystalline cellulose, an attriting agent which is relatively insoluble in water and optionally a protective colloid;
• US 6,117,474 discloses a composition containing a fine cellulose and a water-insoluble calcium material.
• the compositions are prepared by cogrinding an aqueous suspension of cellulose particles and calcium particles.
• a water soluble gum and/or hydrophilic substance may be incorporated in order to prevent re-aggregation of the fine cellulose and water-insoluble calcium material upon drying.
• US 6,270,830 discloses a stabilizer for meat products comprising fine cellulose and a gelling agent.
• the stabilizer may contain a potassium or calcium salt such as insoluble calcium carbonate, to control gelling.
• a method has now been found for preparing a colloidal microcrystalline cellulose/hydrocolloid composition in which the hydrocoUoid has a heterogeneous distribution of linkages and is more intimately mixed with and closely bound to the microcrystalline cellulose than has previously been possible. This result is accomplished by shearing a high solids mixture of the microcrystalline cellulose and the hydrocoUoid by vigorously kneading in the presence of an anti-slip agent.
• composition of this invention may be the moist attrited microcrystalline cellulose/hydrocolloid solid recovered from the kneading process; or it may be the dried residue thereof prepared by removing moisture from the moist solid, the latter being preferred for storage, shipment and subsequent use in preparing microcrystalline cellulose based dispersions.
• the compositions have a mean particle size, when measured as described below, of less than about 10 microns.
• compositions comprising microcrystalline cellulose and a hydrocoUoid.
• the compositions are prepared by (a) combining microcrystalline cellulose wetcake, a hydrocoUoid and an anti-slip agent prior to uniform swelling of the hydrocoUoid, and (b) shearing the combination.
• compositions are characterized by a mean particle size smaller than has previously been achievable in MCC/hydrocolloid compositions and a unique particle size distribution depending upon the hydrocolloid(s) employed.
• hydrocolloids include: seaweed polysaccharides such as carrageenan, agar, furcellaran, alginate and alginate derivatives such as propylene glycol alginate and monovalent salts of alginates such as the potassium and sodium salts, plant gums including galactomannans such as guar, locust bean gum, and tara; carboxymethyl guar, carboxymethyl locust bean gum; glucomannans such as konjac; tamarind seed; polysaccharide; pectin; karaya; acacia; tragacanth; bacterial polysaccharides such as xanthan and pullulan; gellan and wellan; cellulose gums; alkyl cellulose ethers including hydroxypropylmethyl cellulose, hydroxyeth
• the carrageenans may include mu, kappa, kappa-2, nu, iota, lambda, theta and mixtures thereof.
• the carrageenan may be processed with no, low, or high levels of alkali.
• the carrageen may include refined, semi-refined, or unrefined grades and mixtures thereof.
• Preferred hydrocolloids include alginates and carrageenans. Of these, iota carrageenan and sodium alginate are especially preferred.
• Blends of hydrocolloids may be employed particularly blends of iota carrageenan or sodium alginate and a minor portion of other hydrocolloids such as xanthan or pectic substances so long as the anti-slip agent can interact sufficiently to retard hydration of the hydrocoUoid blend in the presence of the microcrystalline cellulose wetcake to enable sufficient mechanical energy transfer under shearing to produce the co-attrited colloidal MCC/ hydrocoUoid.
• natural hydrocolloids As used herein "natural” means present in or produced by nature and includes hydrocolloids recovered from a biological source such as plants or bacteria or microbial fermentation.
• Suitable feedstocks include, for example, wood pulp such as bleached sulfite and sulfate pulps, corn husks, bagasse, straw, cotton, cotton linters, flax, kemp, ramie, fermented cellulose, etc.
• microcrystalline cellulose and hydrocoUoid may be varied over a wide range depending upon the properties desired in the final composition. For most applications the ratio should be equal to from 50/50 to 90/10 more preferably from 70/30 to 85/15 parts by weight.
• the anti-slip agent is a non-lubricant material which functions in combination with the hydrocoUoid.
• the anti-slip agent is employed in an amount sufficient to reduce slippage of the product admixture in the work zones of the equipment during processing, ie. between the rotating screw elements as well as between the extruder screw elements and the extruder barrel itself in a twin screw extruder during mechanical processing of the admixture.
• the anti-slip agent may be any inorganic salt which is essentially completely soluble in water.
• Aqueous soluble inorganic salts which may be used include, for example, sodium chloride, potassium chloride, calcium chloride, calcium lactate, calcium tartrate, calcium citrate, calcium monophosphate and magnesium chloride. Of these divalent salts are preferred. Calcium chloride is especially preferred.
• the amount of inorganic salt depends upon the valency of the salt and the hydrocoUoid involved. The minimum amount is that which is sufficient to produce a non-slippery environment with sufficient friction to transform the MCC aggregates into a colloidal form. If too much salt is used this results in too much friction, increasing the temperature thereby resulting in degradation of the hydrocoUoid. In general an amount of from about 0.8% to about 3.0% by weight based on the total weight of solids may be used. In one embodiment which uses sodium alginate as the hydrocoUoid and calcium chloride as the inorganic salt the amount of calcium chloride salt added is within the range 0.8% to 2.0% by weight preferably 1.0% to 1.5% for an 85:15 weight ratio of microcrystalline cellulose to alginate.
• the added calcium chloride salt is within the range 1.0% to 3.0% by weight, preferably 2.0 to 2.5% for an 85:15 ratio of microcrystalline cellulose to carrageenan. Some amount of the salt generally remains in the final composition.
• a divalent salt such as calcium
• CA ++ is from about 0.18 to 3.5%) based on the total weight of the powdered composition. This includes any amount of calcium ions associated with the hydrocoUoid employed and may, therefore, be higher than the amount of ions in the anti-slip agent employed in the process. The amount of cation present is determined by the atomic absorption test method described below.
• the process of the present invention uses as the starting material a hydrolyzed microcrystalline cellulose wetcake which, as indicated above, contains 40- 60%) by weight water.
• the hydrocoUoid in the form of a dry powder is added to the wetcake with mixing. Only a limited amount of water is available to wet, and swell, the hydrocoUoid powder in the high solids mixture of microcrystalline cellulose wetcake and added hydrocoUoid powder.
• a solution of the inorganic salt is added. It is an important aspect of the present invention that the salt addition occurs prior to uniform wetting and swelling of the hydrocoUoid powder.
• shear force refers to an action resulting from applied force that causes or tends to cause two contiguous parts of a mixture to slide relative to each other in a direction generally parallel to their plane of contact.
• the hydrocoUoid microcrystalline cellulose mixture no longer responds in a slippery manner but is capable of transferring the shear force applied to the mixture as mechanical energy to communite the microcrystalline cellulose aggregates.
• the amount of force applied must be sufficient to force association between the microcrystalline cellulose particles and the hydrocoUoid.
• the mixture remains slippery and the shear force is primarily dissipated as mechanical energy by sliding action rather than transferred to comminute the microcrystalline cellulose aggregates. If too much salt is added, the resistance to shear is very high and the hydrocoUoid in the mixture is subject to degradation due to localized heating.
• the resulting sheared material is dispersed in water, homogenized and spray dried to produce the final composition of the present invention.
• the present invention utilizes as one of the starting materials a hydrolyzed cellulose wetcake (i.e., the undried mass produced when a source of cellulose, preferably alpha cellulose in the form of pulp from fibrous plant materials, has been treated with a mineral acid and then washed to remove the acid and byproducts) generally containing about 40 to about 60 percent moisture to which a hydrocoUoid is added.
• An anti-slip agent such as an aqueous solution of a soluble salt is added to the mixture of the microcrystalline cellulose wetcake and hydrocoUoid before the hydrocoUoid has had an opportunity to uniformly swell.
• the mixture of partially hydrated hydrocoUoid and microcrystalline cellulose particles is then subjected to high solids shearing wherein the partially swollen hydrocoUoid facilitates attrition of the microcrystalline cellulose to provide colloidal particles. If the hydrocoUoid were allowed to uniformly swell prior to shearing, the swollen hydrocoUoid would be too slippery to be processed and there would be insufficient energy transfer during shearing to provide the necessary particle-to-particle abrasion forces required to reduce the microcrystalline particles to a consistent sub-micron size during the attrition step.
• the moisture content may be adjusted as desired to produce the consistency desired for attrition of the blend and adjusted as needed during attrition to maintain the desired consistency.
• the moisture present in the wetcake is generally sufficient. The use of excess water is to be avoided as it will tend to reduce the particle-to-particle abrasion forces which are necessary to reduce the microcrystalline cellulose particles to a consistent sub-micron size.
• the wet blend is then attrited preferably as a high-solids wet blend under high shear high solids mixing conditions, in which the microcrystalline cellulose is ground into ultra-fine sub-micron sized particles which on dispersion are coUoidally stable.
• the colloidal stability is further facilitated by inclusion of the protective hydrocoUoid.
• the protective hydrocolloids may perform one or more of several functions. They act as a barrier between and/or around the microcrystalline cellulose particles, presumably by attaching to or replacing the hydrogen bonding forces between them, and thus form a barrier between such particles to prevent them from hornifying. Secondly they act as dispersion aids to facilitate dispersion and rehydration of the microcrystalline cellulose particles when dried solid compositions of microcrystalline cellulose are redispersed. In addition, they may help in suspending and/or altering the rheological properties of the suspension.
• Reduction of microcrystalline cellulose to colloidal particle size is preferably carried out by high solids, wet shearing of the blend of microcrystalline cellulose, inorganic salt solution and protective colloid.
• a standard extruder preferably with multiple screws, is a preferred means for reducing microcrystalline cellulose particle size.
• Other standard equipment may also be used for wet shearing operations, such as planetary mixers, for example Hobart mixers and roll mills, particularly those having three or more rolls.
• the equipment used provide high shearing action and provide intense rubbing, abrasive action on the microcrystalline cellulose, for example by forcing the mixture through passages of limited cross section such as those found in perforated plates of extruders and various other mixing equipment, or other passages of limited clearance such as between rolls of roller mills.
• the extrusion process is preferred for its ease of operation in high solids, high throughput processing and for its efficacy in yielding very fine particles of microcrystalline cellulose.
• the first step comprises blending together unattrited microcrystalline cellulose and the hydrocoUoid.
• the anti-slip agent is added prior to high shear kneading. As indicated above it is also possible to combine the microcrystalline cellulose and the anti-slip agent prior to addition of the hydrocoUoid.
• the wet blend is then subjected to high shear kneading for a time and under shear forces sufficient to reduce the microcrystalline cellulose to a particle size in which about 80% to 100%, advantageously about 90% to 100%, of the microcrystalline cellulose has a particle size not greater than 1 micrometer and is coUoidally stable when dispersed in aqueous media.
• the hydrocoUoid is closely bound to the microcrystalline cellulose.
• the moist attrited microcrystalline cellulose composition resulting from the extrusion or other suitable kneading process may be recovered and then dispersed as a stabilizer/suspending agent for suspension and dispersions and/or may be further processed, dried and then dispersed for such uses.
• the further processing steps, if utilized, may involve preparing an initial dispersion, homogenizing the resulting dispersion, drying it, for example, by spray drying or other suitable means, all of which are within the skill of the art.
• compositions of this invention thus comprise an ultra-fine attrited microcrystalline cellulose composition comprising an anti-slip agent and microcrystalline cellulose particles which have a particle size as described above and a protective hydrocoUoid, in which the weight ratio of microcrystalline cellulose to protective colloid is in the range of about 50:50 to about 90:10, preferably from 70:30 to 85:15.
• the ultra fine coUoidally stable microcrystalline cellulose/hydrocolloid product of this invention is utilized in dispersions, emulsions, suspensions and the like in an amount of from about 0.05-15 weight percent, advantageously 0.03 to 5 weight percent, preferably from about 0.05-3 weight percent, and is used as a filler or bulking agent, in an amount of about 1-15 weight percent, based on the final product. For food applications, 0.05-15 weight percent may suitably be used.
• the products prepared by the present process differ from those prepared by prior art processes. As compared to the products prepared by the processes of the Kamada et al and Nenables et al patents discussed above in which a solid attriting aid is used, the products of the present invention exhibit molecular distribution of the inorganic salt throughout the hydrocolloid/microcrystalline composition rather than in the form of fine inorganic particulates. The heterogeneous distribution of linked hydrocoUoid closely bound with the colloidal microcrystalline cellulose provides for unique rheological behavior of the re-dispersed powder. As compared to the process of Tuason et al.
• the products of the present invention exhibit finer colloidal particle size with tightly bound and heterogeneous linked alginate polymer due to high solids wet shearing of the microcrystalline cellulose wetcake and the partially swollen hydrocoUoid in the presence of the antislip agent.
• compositions of the present invention are "coattrited" meaning that the MCC and the hydrocoUoid are combined prior to application of high shear forces to the combination. They are characterized by physical properties not heretofore achievable.
• compositions contain at least 70%> MCC and have a mean particle size of less than 10 microns.
• particle size refers to the value obtained by the test procedure described below.
• Prefered compositions have a particle size distribution (again determined by the test procedure described below) which depends on the hydrocolloid(s) used. Specifically,
• the products of the present invention can be used where colloidal grades of MCC are currently used including retortable chocolate beverages, bake stable bakery fillings, frozen desserts, aerated food systems, and salad dressings. These products are particularly suited for UHT-processed beverages, dairy and nondairy, such as those containing fresh soy protein or soy isolate, cocoa powder, and nutritional additives such as vitamins and minerals.
• this new colloidal MCC product extends product functionality to open up new opportunities for colloidal MCC. New product applications are due to the new and/or improved properties of the product.
• compositions can be used at low levels but with more process latitude since the range of effectiveness is broader so the amount is not narrowly critical. Dry mix products (instant sauces, gravies, soups, instant cocoa drinks, etc.), low pH dairy systems (sour cream/yogurt, yogurt drinks, stabilized frozen yogurt), baked goods (pie/pastry fillings), beverages (citrus flavored drinks, etc.), and products labeled all are areas of application.
• compositions may be used as thickeners, in foams, creams and lotions for personal care (skin, hair) applications, and as suspending agents, for use with pigments and fillers in ceramics, colorants, cosmetics, and oral care and in industrial applications such as ceramics, delivery systems for pesticides including insecticides and in other agricultural products.
• a dispersion was prepared with a Waring Blender (700 series), using a 1,000 ml bowl, at a speed of 18,000 to 19,000 rpm controlled by a Powerstat transformer which permits increasing of the Waring Blender speed gradually to avoid splashing. 1.
• the mean particle size and the particle size distribution were measured using a Horiba
• LA-910 (available from Horiba Instruments, Inc., Irvine, Calif.) static light scattering particle size distribution analyzer.
• HCI hydrochloric acid
• Oxidant Flow 10.0 L/min.
• % Calcium (weight of calcium (mg)/sample weight (mg) • (100 - % LOD/100)) 100
• % Calcium chloride % calcium • (110.98/40.08) III.
• Bake (Heaf) Stability was determined by measuring shape retention by the following procedure. Shape retention is defined as the capacity of a fruit filling preparation to retain its initial shape and volume after being baked for a definite amount of time at a given temperature. A defined volume of fruit filling preparation (approx 35 g) is placed in a standardized ring (3.5 cm), which is placed on a paper graduated with concentric circles. The fruit filling is baked for a defined period of time at a specific temperature (usually 10 minutes at 400°F.) in a ventilated oven. After the heat treatment, the spread of the fruit filling is measured. The spread is expressed in a percentage [(Final diameter -initial diameter)/initial diameter x 100].
• MCC microcrystalline cellulose
• a water dispersible colloidal MCC powder having a very fine colloidal particle size distribution was obtained.
• Particle size analysis by laser light diffraction showed that the powder had a mean particle size of 5.33 microns and a particle size distribution of 85%) of the particles less than 3.5 microns.
• its 2.6% dispersion exhibited an initial Brookfield viscosity of 1,100 cps and a viscosity of 1,150 cps when retested after 24 hours.
• MCC microcrystalline cellulose
• MCC microcrystalline cellulose
• iota carrageenan a solids content ranging from 38-44%
• 40 grams of a 30% solution of CaCl 2 was added and mixed for several minutes.
• the admixture was passed through a co rotating twin-screw extruder several times to shear the admixture and comminute the microcrystalline aggregates.
• the resulting consistency of the extrudate was not slippery thereby enabling it to be subjected to a high work profile which facilitated the formation of colloidal microcrystalline cellulose particles.
• a water dispersible colloidal MCC powder having a very fine colloidal particle size distribution was obtained. Particle size analysis by laser light diffraction showed that the powder had a mean particle size of 4.27 microns. When dispersed in water, its 2.6%) dispersion exhibited an initial viscosity of 1,700 cps and a set-up viscosity of 2,450 cps when retested after 24 hours suggesting an effective interaction that is, a good gel network, between the MCC and the iota carrageenan. A 0.5%) level of this 85/15 microcrystalline cellulose/iota carrageenan provided a stable cocoa suspension in a retortable nutraceutical chocolate beverage and a UHT processed soy protein-based chocolate beverage.
• MCC microcrystalline cellulose
• the resulting consistency of the extrudate was still slippery and thus, the necessary friction or work profile in the extruder was not obtained to mechanically disintegrate the MCC aggregates into ultra fine particles.
• Microscopic evaluation of the extrudate revealed that the MCC particles were large and unattrited thus, they were not colloidal.
• the amount of calcium salt added was insufficient to compete with the carrageenan for water hence, allowing the carrageenan gum to solvate further.
• MCC microcrystalline cellulose
• iota carrageenan a solids content ranging from 38-44%>
• 75 grams of a 30%> solution of CaCl 2 was added and mixed for several minutes.
• the admixture was passed through a co rotating twin-screw extruder several times to shear the admixture and comminute the microcrystalline aggregates.
• the resulting consistency of the extrudate was not slippery thereby enabling it to be subjected to a high work profile which facilitated the formation of colloidal microcrystalline cellulose particles.
• Gaulin homogenizer at 2,500 psi and spray dried to form a powder The spray drying was performed as follows: The homogenized slurry was fed to a 3 foot (0.9144 m) Bowen spray dryer utilizing nozzle atomization 0.1 inch (0.00254 m) opening. The slurry was fed to the dryer by means of a variable feed Moyno pump at a rate to provide the desired outlet temperature. The operating inlet/outlet air temperature of the spray dryer was about 195°C/95°C. The spray drying conditions were regulated depending upon feed properties such as viscosity and resulting dried product characteristics and subsequent yield.
• a water dispersible colloidal MCC powder having a very fine colloidal particle size distribution was obtained.
• its 2.6%> dispersion exhibited an initial viscosity of 2,000 cps and a set up viscosity of 12,900 cps when retested after 24 hours suggesting an effective interaction that is, a good gel network between the MCC and the iota carrageenan.
• a sweetened yogurt prepared using 0.25 wt%> of this 70/30 microcrystalline celluose/iota carrageenan powder had a smooth consistency and glossy texture.
• the 70/30 MCC/iota-based product was stable as it maintained its smooth and glossy texture.
• MCC microcrystalline cellulose
• a water dispersible colloidal MCC powder having a very fine colloidal particle size distribution was obtained. Particle size analysis by laser light diffraction showed that the powder had a mean particle size of 6.04 microns. When dispersed in water, its 2.6%o dispersion exhibited an initial viscosity of 1,675 cps and a set up viscosity after 24 hours of 1,725 cps.
• MCC microcrystalline cellulose
• a water dispersible colloidal MCC powder having a very fine particle size distribution in which 50% of the particles were below 3.5 microns was obtained.
• its 2.6% dispersion exhibited an initial viscosity of 725 cps and a set-up viscosity of 3.350 cps.
• the 85/15 MCC/ kappa carrageenan used at 0.10%> provided a stable cocoa suspension.
• EXAMPLE VI 70/30 MCC/HM PECTIN
• MCC microcrystalline cellulose
• HM high methoxyl
• the resulting consistency of the extrudate was not slippery thereby enabling it to be subjected to a high work profile which facilitated the formation of colloidal microcrystalline cellulose particles.
• 315.1 grams of the MCC/iota carrageenan extrudate was dispersed in 2,684.9 grams of distilled water at about 160°F. 3 grams of K CO 3 was added and mixed for several minutes to adjust the pH to 5.0-5.4.
• the resulting slurry was passed through a Manton Gaulin homogenizer at 2,500 psi and spray dried to form a powder.
• the spray drying was performed as follows: The homogenized slurry was fed to a 3 foot (0.9144 m) Bowen spray dryer utilizing nozzle atomization 0.1 inch (0.00254 m) opening.
• the slurry was fed to the dryer by means of a variable feed Moyno pump at a rate to provide the desired outlet temperature.
• the operating inlet/outlet air temperature of the spray dryer was about 195°C/95°C.
• the spray drying conditions were regulated depending upon feed properties such as viscosity and resulting dried product characteristics and subsequent yield.
• a water dispersible colloidal MCC powder having a very fine particle size distribution was obtained.
• Particle size analysis by laser light diffraction of its 2.6% dispersion showed that it had a median particle size of 6.56 microns and a mean particle size of
• the 70/30 MCC HM pectin used at 0.33% produced good stabilization.
• MCC microcrystalline cellulose
• PGA propylene glycol alginate
• DE high degree of esterification
• 65 grams of a 30%) solution of CaCl 2 was added and mixed for several minutes.
• the admixture was passed through a co rotating twin-screw extruder several times to shear the admixture and comminute the microcrystalline aggregates.
• the resulting consistency of the extrudate was not slippery thereby enabling it to be subjected to a high work profile which facilitated the formation of colloidal microcrystalline cellulose particles.
• a water dispersible colloidal MCC powder having a very fine particle size distribution was obtained.
• Particle size analysis by laser light diffraction of its 2.6%> dispersion showed that it had a median particle size of 5.87 microns and a mean particle size of 7.40 microns.
• the 70/30 MCC/PGA used at 0.35% produced good stabilization.
• MCC microcrystalline cellulose
• the spray drying was performed as follows: The homogenized slurry was fed to a 3 foot (0.9144 m) Bowen spray dryer utilizing nozzle atomization 0.1 inch (0.00254 m) opening. The slurry was fed to the dryer by means of a variable feed Moyno pump at a rate to provide the desired outlet temperature. The operating inlet/outlet air temperature of the spray dryer was about 195°C/95°C. The spray drying conditions were regulated depending upon feed properties such as viscosity and resulting dried product characteristics and subsequent yield.
• a water dispersible colloidal MCC powder having a very fine particle size distribution with 21%) of the particles below 3.5 microns was obtained.
• its 2.6%o dispersion exhibited an initial viscosity of 725 cps and a set-up viscosity of
• MCC microcrystalline cellulose
• the resulting consistency of the extrudate was not slippery thereby enabling it to be subjected to a high work profile which facilitated the formation of colloidal microcrystalline cellulose particles.
• 343.5grams of the MCC/iota carrageenan/HM pectin extrudate was dispersed in 2,656.6 grams of distilled water at about 160°F.
• the resulting slurry was passed through a Manton Gaulin homogenizer at 2,500 psi and spray dried to form a powder.
• the spray drying was performed as follows: The homogenized slurry was fed to a 3 foot (0.9144 m) Bowen spray dryer utilizing nozzle atomization 0.1 inch (0.00254 m) opening.
• the slurry was fed to the dryer by means of a variable feed Moyno pump at a rate to provide the desired outlet temperature.
• the operating inlet/outlet air temperature of the spray dryer was about 195°C/95°C.
• the spray drying conditions were regulated depending upon feed properties such as viscosity and resulting dried product characteristics and subsequent yield.
• a water dispersible colloidal MCC powder having a very fine particle size distribution with 26% of the particles below 3.5 microns was obtained. When dispersed in water, its 2.6%o dispersion exhibited an initial viscosity of 450 cps and a set-up viscosity of 700 cps.
• a fruit filling composition was prepared from the following components. All amounts are in parts by weight. In this Example, the following materials were used:
• the GRLNSTED LA410 and MCC/Sodium Alginate were dry blended and then dispersed in water using high shear mixing for 7 minutes. The sample was then heated
• Brix was determined using a refractometer.
• the calcium lactate and citric acid solutions were added sequentially.
• the fruit filling was poured into jars.
• Hot viscosity was measured using a Brookfield RVT #4 spindle, 10 ⁇ m after 1 minute. The samples were cooled to room temperature and refrigerated prior to testing for gel strength and bake stability.

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