WO2006127810A2 - Bacterial cellulose-containing formulations and method of producing effective bacterial cellulose-containing formulations - Google Patents

Bacterial cellulose-containing formulations and method of producing effective bacterial cellulose-containing formulations Download PDF

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Publication number
WO2006127810A2
WO2006127810A2 PCT/US2006/020080 US2006020080W WO2006127810A2 WO 2006127810 A2 WO2006127810 A2 WO 2006127810A2 US 2006020080 W US2006020080 W US 2006020080W WO 2006127810 A2 WO2006127810 A2 WO 2006127810A2
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Prior art keywords
gum
bacterial cellulose
formulation
precipitation agent
product
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PCT/US2006/020080
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English (en)
French (fr)
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WO2006127810A3 (en
WO2006127810A8 (en
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Zhifa Yang
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Zhifa Yang
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Priority claimed from US11/135,065 external-priority patent/US20070027108A1/en
Priority claimed from US11/135,077 external-priority patent/US8053216B2/en
Priority to BRPI0613298-7A priority Critical patent/BRPI0613298B1/pt
Priority to CA002609677A priority patent/CA2609677A1/en
Priority to JP2008513669A priority patent/JP2008541728A/ja
Priority to MX2007014697A priority patent/MX2007014697A/es
Application filed by Zhifa Yang filed Critical Zhifa Yang
Priority to KR1020077029842A priority patent/KR101234471B1/ko
Priority to CN200680022042.9A priority patent/CN101203615B/zh
Priority to AU2006250004A priority patent/AU2006250004B2/en
Publication of WO2006127810A2 publication Critical patent/WO2006127810A2/en
Publication of WO2006127810A3 publication Critical patent/WO2006127810A3/en
Priority to NO20076536A priority patent/NO20076536L/no
Publication of WO2006127810A8 publication Critical patent/WO2006127810A8/en

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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38Cellulose; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/14Hemicellulose; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08Cellulose derivatives
    • C08L1/26Cellulose ethers
    • C08L1/28Alkyl ethers
    • C08L1/284Alkyl ethers with hydroxylated hydrocarbon radicals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00

Definitions

  • the present invention relates generally to a new method to produce formulations of bacterial cellulose that exhibit improved viscosity-modifying properties particularly with low energy applied to effectuate viscosity changes therewith.
  • a method includes the novel co- precipitation with a water soluble co-agent that permits precipitation in the presence of excess alcohol to form an insoluble fiber that can than be utilized as a thickener or suspension aid without the need to introduce high energy mixing.
  • Such bacterial cellulose properties have been available in the past but only through highly labor and energy intensive processes.
  • Such an inventive method as now proposed thus provides a bacterial cellulose-containing formulation that exhibits not only properties as effective as those for previous bacterial celluloses, but, in some ways, improvements to such previous types. Certain end-use compositions and applications including these novel bacterial cellulose-containing formulations are also encompassed within this invention.
  • Bacterial cellulose is a broad category of polysaccharides that exhibit highly desirable properties, even though such compounds are essentially of the same chemical structure as celluloses derived from plant material. As the name purports, however, the source of these polysaccharides are bacterial in nature (produced generally by microorganisms of the Acetobacter genus) as the result of fermentation, purification, and recovery thereof.
  • Such bacterial cellulose compounds are comprised of very fine cellulosic fibers having very unique dimensions and aspect ratios (diameters of from about 40 to 100 nm each and lengths of from 0.1 to 15 microns) in bundle form (with a diameter of 0.1 to 0.2 microns on average),
  • Such an entangled bundle structure forms a reticulated network structure that facilitates swelling when in aqueous solution thereby providing excellent three-dimensional networks.
  • the three- dimensional structures effectuate proper and desirable viscosity modification as well as suspension capabilities through building a yield-stress system within a target liquid as well as excellent bulk viscosity.
  • Such a result thus permits highly effective suspension of materials (such as foodstuffs, as one example) that have a propensity to settle over time out of solution, particularly aqueous solutions.
  • materials such as foodstuffs, as one example
  • bacterial cellulose formulations aid in preventing settling and separation of quick-preparation liquid foodstuffs (i.e., soups, chocolate drinks, yogurt, juices, dairy, cocoas, and the like), albeit with the need to expend relatively high amounts of energy through mixing or heating to initially reach the desired level of suspension for such foodstuffs .
  • the resultant fibers are insoluble in water and, with the capabilities noted above, exhibit polyol- and water-thickening properties.
  • One particular type of bacterial cellulose, microfibrillated cellulose is normally provided in an uncharged state and exhibits the ability to associate without any added influences.
  • the resultant systems will themselves exhibit high degrees of instability, particularly over time periods associated with typical shelf life requirements of foodstuffs.
  • CMC carboxymethylcellulose
  • this invention encompasses a method for the production of a bacterial cellulose-containing formulation comprising the steps of a) providing a bacterial cellulose product through fermentation; b) optionally lysing the bacterial cells from the resultant bacterial cellulose product; c) mixing said resulting bacterial cellulose of either step "a" or "b” product with a polymeric thickener selected from the group consisting of at least one charged cellulose ether, at least one precipitation agent, and any combination thereof; and d) co-precipitating the mixture of step "c" with a water-miscible nonaqueous liquid (such as, as one non-limiting example, an alcohol).
  • a water-miscible nonaqueous liquid such as, as one non-limiting example, an alcohol
  • the possible charged cellulose ether of step “c” is a compound utilized to disperse and stabilize the reticulated network in the final end-use compositions to which such a bacterial cellulose- containing formulation is added.
  • the charged compounds facilitate, as alluded to above, the ability to form the needed network of fibers through the repulsion of individual fibers.
  • the possible precipitation agent of step “c” is a compound utilized to preserve the functionality of the reticulated bacterial cellulose fiber during drying and milling.
  • Examples of such charged cellulose ethers include such cellulose-based compounds that exhibit either an overall positive or negative and include, without limitation, any sodium carboxymethylcellulose (CMC), cationic hydroxyethylcellulose, and the like.
  • the precipitation (drying) agent is selected from the group of natural and/or synthetic products including, without limitation, xanthan products, pectin, alginates, gellan gum, welan gum, diutan gum, rhamsan gum, carrageenan, guar gum, agar, gum arabic, gum ghatti, karaya gum, gum tragacanth, tamarind gum, locust bean gum, and the like.
  • a precipitation (drying) agent is included.
  • one more specific method encompassed within this invention comprises the steps of a) providing a bacterial cellulose product through fermentation; b) optionally lysing the bacterial cells from the bacterial cellulose product; c) mixing said resulting bacterial cellulose product of either step "a” or step “b” with a biogum (which if incorporated as a fermentation broth has had the bacterial cells preferably lysed there from); and d) co-precipitating the mixture of step "c" with a water-miscible nonaqueous liquid.
  • such a specific method may comprise the steps of a) providing a bacterial cellulose product through fermentation; b) mixing said bacterial cellulose product with a biogum; c) co-lysing the mixture of step "b” to remove bacterial cells therefrom; and d) co-precipitating the mixture of step "c" with a water-miscible nonaqueous liquid.
  • the resultant coprecipitated product will be in the form of a presscake that can then be dried and the particles obtained thereby may then be milled to a desired particle size.
  • the particles may then be blended with another hydrocolloid, such as carboxymethylcellulose (CMC), to provide certain properties.
  • CMC carboxymethylcellulose
  • an inventive product of this development would be defined as a bacterial cellulose- containing formulation comprising at least one bacterial cellulose material and at least one polymeric thickener selected from the group consisting of at least one charged cellulose ether, at least precipitation agent selected from the group consisting of xanthan products, pectin, alginates, gellan gum, welan gum, diutan gum, rhamsan gum, carrageenan, guar gum, agar, gum arabic, gum ghatti, karaya gum, gum tragacanth, tamarind gum, locust bean gum, and the like, and any mixtures thereof, wherein said formulation exhibits a viscosity capability of at least 300 cps and a yield stress measurement of 1.0 dyne/cm 2 when introduced in an amount of at most 0.36% by weight of a 500 mL sample of water and after application of at most 2 passes at 1500 psi in an extensional homogenizer.
  • the formulation of bacterial cellulose and xanthan produced thereby has the distinct advantage of facilitating activation without any labor- or energy-intensive activation required.
  • Another distinct advantage of this overall method is the ability to collect the resultant bacterial cellulose-containing formulation through precipitation with isopropyl alcohol, whether with a charged cellulose ether or a precipitation (drying) agent present therein.
  • the alcohol-insoluble polymeric thickener such as xanthan or sodium CMC
  • the polymeric thickener actually helps associate and dewater the cellulosic fibers upon the addition of a nonaqueous liquid (such as preferably a lower alkyl alcohol), thus resulting in the collection of substantial amounts of the low-yield polysaccharide during such a co-precipitation stage.
  • a nonaqueous liquid such as preferably a lower alkyl alcohol
  • the avoidance of substantial amounts of water during the purification and recovery steps thus permits larger amounts of the bacterial cellulose to be collected ultimately.
  • the highest amount of fermented bacterial cellulose can be collected, thus providing the high efficiency in production desired, as well as the avoidance of, as noted above, wastewater and multiple passes of dewatering and re- slurrying typically required to obtain such a resultant product.
  • a drying agent in particular, as one non-limiting example, a xanthan product, as a coating over at least a portion of the bacterial cellulose fiber bundles, appears to provide the improvement in activation requirements when introduced within a target end use composition.
  • a drying agent in particular, as one non-limiting example, a xanthan product, as a coating over at least a portion of the bacterial cellulose fiber bundles.
  • MFC microfibrillated cellulose
  • bacterial cellulose-containing formulation is intended to encompass a bacterial cellulose product as produced by the inventive method and thus including xanthan product coating at least of the portion of the resultant bacterial cellulose fiber bundles.
  • formulation thus is intended to convey that the product made therefrom is a combination of bacterial cellulose and xanthan produced in such a manner and exhibiting such a resultant structure and configuration.
  • bacterial cellulose is intended to encompass any type of cellulose produced via fermentation of a bacteria of the genus Acetobacter and includes materials referred popularly as microfibrillated cellulose, reticulated bacterial cellulose, and the like.
  • bacterial cellulose may be used as an effective rheological modifier in various compositions.
  • Such materials when dispersed in fluids, produce highly viscous, thixotropic mixtures possessing high yield stress. Yield stress is a measure of the force required to initiate flow in a gel -like system. It is indicative of the suspension ability of a fluid, as well as indicative of the ability of the fluid to remain in situ after application to a vertical surface.
  • such rheological modification behavior is provided through some degree of processing of a- mixture of the bacterial cellulose in a hydrophilic solvent, such as water, polyols (e.g., ethylene glycol, glycerin, polyethylene glycol, etc.), or mixtures thereof.
  • a hydrophilic solvent such as water, polyols (e.g., ethylene glycol, glycerin, polyethylene glycol, etc.), or mixtures thereof.
  • This processing is called “activation” and comprises, generally, high pressure homogenization and/or high shear mixing.
  • the inventive bacterial cellulose-containing formulations of the invention have been found to activate at low energy mixing. Activation is a process in which the 3- dimensional structure of the cellulose is modified such that the cellulose imparts functionality to the base solvent or solvent mixture in which the activation occurs, or to a composition to which the activated cellulose is added.
  • Functionality includes providing such properties as thickening, imparting yield stress, heat stability, suspension properties, freeze-thaw stability, flow control, foam stabilization, coating and film formation, and the like.
  • the processing that is followed during the activation process does significantly more than to just disperse the cellulose in base solvent. Such processing "teases apart" the cellulose fibers to expand the cellulose fibers.
  • the bacterial cellulose-containing formulation may be used in the form of a wet slurry (dispersion) or as a dried product, produced by drying the dispersion using well-known drying techniques, such as spray-drying or freeze-drying to impart the desired rheological benefits to a target fluid composition.
  • the activation of the bacterial cellulose expands the cellulose portion to create a reticulated network of highly intermeshed fibers with a very high surface area.
  • the activated reticulated bacterial cellulose possesses an extremely high surface area that is thought to be at least 200-fold higher than conventional microcrystalline cellulose (i.e., cellulose provided by plant sources).
  • the bacterial cellulose utilized herein may be of any type associated with the fermentation product of Acetobacter genus microorganisms, and was previously available, as one example, from CPKelco U.S. under the tradename CELLULON®. Such aerobic cultured products are characterized by a highly reticulated, branching interconnected network of fibers that are insoluble in water.
  • Dry reticulated bacterial cellulose can be produced using drying techniques, such as spray-drying or freeze-drying, that are well known.
  • Acetobacter is characteristically a gram-negative, rod shaped bacterium 0.6-0.8 microns by 1.0-4 microns. It is a strictly aerobic organism; that is, metabolism is respiratory, not fermentative. This bacterium is further distinguished by the ability to produce multiple poly ⁇ - 1,4-glucan chains, chemically identical to cellulose.
  • the microcellulose chains, or microfibrils, of reticulated bacterial cellulose are synthesized at the bacterial surface, at sites external to the cell membrane. These microfibrils generally have cross sectional dimensions of about 1.6 nm by 5.8 nm.
  • the microfibrils at the bacterial surface combine to form a fibril generally having cross sectional dimensions of about 3.2 nm by 133 nm.
  • the small cross sectional size of these Acetobacter-pvoduced fibrils, together with the concomitantly large surface and the inherent hydrophilicity of cellulose, provides a cellulose product having an unusually high capacity for absorbing aqueous solutions.
  • Additives have often been used in combination with the reticulated bacterial cellulose to aid in the formation of stable, viscous dispersions. The aforementioned problems inherent with purifying and collecting such bacterial cellulose have led to the determination that the method employed herein provides excellent results to the desired extent.
  • the first step in the overall process is providing any amount of the target bacterial cellulose in fermented form.
  • the production method for this step is described above.
  • the yield for such a product has proven to be very difficult to generate at consistently high levels, thus it is imperative that retention of the target product be accomplished in order to ultimately provide a collected product at lowest cost.
  • Ly sing of the bacterial cells from the bacterial cellulose product is accomplished through the introduction of a caustic, such as sodium hydroxide, or any like high pH (above about 12.5 pH, preferably) additive in an amount to properly remove as many expired bacterial cells as possible from the cellulosic product. This may be followed in more than one step if desired. Neutralizing with an acid is then typically followed. Any suitable acid of sufficiently low pH and molarity to combat (and thus effectively neutralize or reduce the pH level of the product as close to 7.0 as possible) may be utilized. Sulfuric acid, hydrochloric, and nitric acid are all suitable examples for such a step.
  • a caustic such as sodium hydroxide, or any like high pH (above about 12.5 pH, preferably) additive in an amount to properly remove as many expired bacterial cells as possible from the cellulosic product.
  • Neutralizing with an acid is then typically followed. Any suitable acid of sufficiently low pH and molarity to combat (and thus effectively neutralize or reduce the
  • the cells may be lysed and digested through enzymatic methods (treatment with lysozyme and protease at the appropriate pH).
  • the lysed product is then subjected to mixing with a polymeric thickener in order to effectively coat the target fibers and bundles of the bacterial cellulose.
  • the polymeric thickener must be insoluble in alcohol (in particular, isopropyl alcohol).
  • Such a thickener is either an aid for dispersion of the bacterial cellulose within a target fluid composition, or an aid in drying the bacterial cellulose to remove water therefrom more easily, as well as potentially aid in dispersing or suspending the fibers within a target fluid composition.
  • Proper dispersing aids include, without limitation, CMC (of various types), cationic HEC, etc., in essence any compound that is polymeric in nature and exhibits the necessary dispersion capabilities for the bacterial cellulose fibers when introduced within a target liquid solution.
  • a dispersing aid is CMC, such as CEKOL® available from CP Kelco.
  • Proper precipitation aids include any number of biogums, including xanthan products (such as KELTROL®, KELTROL T®, and the like from CP Kelco), gellan gum, welan gum, diutan gum, rhamsan gum, guar, locust bean gum, and the like, and other types of natural polymeric thickeners, such as pectin, as one non-limiting example.
  • the polymeric thickener is a xanthan product and is introduced and mixed with the bacterial cellulose in a broth form.
  • the commingling of the two products in broth, powder or rehydrated powder form allows for the desired generation of a xanthan coating on at least a portion of the fibers and/or bundles of the bacterial cellulose.
  • the broths of bacterial cellulose and xanthan are mixed subsequent to purification (lysing) of both in order to remove the residual bacterial cells.
  • the broths may be mixed together without lysing initially, but co-lysed during mixing for such purification to occur.
  • the bacterial cellulose will typically be present in an amount from about 0.1% to about 5% by weight of the added polymeric thickener, preferably from about 0.5 to about 3.0%, whereas the polymeric thickener may be present in an amount form 10 to about 900% by weight of the bacterial cellulose.
  • the resultant product is then collected through co-precipitation in a water-miscible nonaqueous liquid.
  • a water-miscible nonaqueous liquid is an alcohol, such as, as most preferred, isopropyl alcohol.
  • alcohols such as ethanol, methanol, butanol, and the like, may be utilized as well, not to mention other water-miscible nonaqeuous liquids, such as acetone, ethyl acetate, and any mixtures thereof. Any mixtures of such nonaqueous liquids may be utilized, too, for such a co-precipitation step.
  • the co- precipitated product is processed through a solid-liquid separation apparatus, allowing for the alcohol-soluble components to be removed, leaving the desired bacterial cellulose-containing formulation thereon.
  • a wetcake form product is collected and then transferred to a drying apparatus and subsequently milled for proper particle size production.
  • Further co-agents may be added to the wetcake or to the dried materials in order to provide further properties and/or benefits
  • co-agents include plant, algal and bacterial polysaccharides and their derivatives along with lower molecular weight carbohydrates such as sucrose, glucose, maltodextrin, and the like.
  • additives that may be present within the bacterial cellulose-containing formulation include, without limitation, a hydrocolloid, polyacrylamides (and homologues), polyacrylic acids (and homologues), polyethylene glycol, poly(ethylene oxide), polyvinyl alcohol, polyvinylpyrrolidones, starch (and like sugar-based molecules), modified starch, animal-derived gelatin, and non-charged cellulose ethers (such as carboxymethylcellulose, hydroxyethylcellulose, and the like).
  • a hydrocolloid polyacrylamides (and homologues), polyacrylic acids (and homologues), polyethylene glycol, poly(ethylene oxide), polyvinyl alcohol, polyvinylpyrrolidones, starch (and like sugar-based molecules), modified starch, animal-derived gelatin, and non-charged cellulose ethers (such as carboxymethylcellulose, hydroxyethylcellulose, and the like).
  • the bacterial cellulose-containing formulations of this invention may then be introduced into a plethora of possible food compositions, including, beverages, frozen products, cultured dairy, and the like; non-food compositions, such as household cleaners, fabric conditioners, hair conditioners, hair styling products, or as stabilizers or formulating agents for asphalt emulsions, pesticides, corrosion inhibitors in metal working, latex manufacture, as well as in paper and non- woven applications, biomedical applications, pharmaceutical excipients, and oil drilling fluids, etc.
  • non-food compositions such as household cleaners, fabric conditioners, hair conditioners, hair styling products, or as stabilizers or formulating agents for asphalt emulsions, pesticides, corrosion inhibitors in metal working, latex manufacture, as well as in paper and non- woven applications, biomedical applications, pharmaceutical excipients, and oil drilling fluids, etc.
  • the fluid compositions including this inventive formulation, prepared as described above, may include such bacterial cellulose-containing formulations in an amount from about 0.01% to about 1% by weight, and preferably about 0.03% to about 0.5% by weight of the total weight of the fluid composition.
  • the ultimately produced bacterial cellulose-containing formulation should impart a viscosity modification to water sample of 500 mL (when added in an amount of at most 0.36% by weight thereof) of at least 300 cps as well as a yield stress measurement within the same test sample of at least 1.0 dynes/cm 2 .
  • Example 1 provides teachings of various methods that are encompassed within this invention.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and
  • the graduated cylinders were then each stored at room temperature (22-25 0 C) for 24 hours to determine if precipitation occurred during that period of time.
  • the phase separations for samples from either the top or the bottom were less than 10% (through visual estimation), thus indicating excellent long-term suspension properties.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% by weight of CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 10 min.
  • the product viscosity and yield stress were 709 cP and 1.96 dynes/cm 2 , respectively.
  • Example 3 MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% by weight of CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 10 min.
  • the product viscosity and yield stress were 635 cP and 1.54 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was then dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 10% CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 10 min.
  • the product viscosity and yield stress were 1242 cP and 4.5 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was then dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% of CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 10 min.
  • the product viscosity and yield stress were 1242 cP and 4.5 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.49 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • a portion of the treated MFC broth was mixed with a given amount of xanthan gum broth (MFC/XG ⁇ 3/1, dry basis) and the resultant mixture was then precipitated with IPA (85%) to form a press cake.
  • the press cake was then dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% by weight of CMC added simultaneously, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosity and yield stress measurements were 1010 cP and 1.76 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.93 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was then dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 5 min.
  • the product viscosity and yield stress were 690 cP and 2.19 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.93 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was then dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, and the composition was then mixed with a Silverson mixer at 8000 rpm for 5 min.
  • the product viscosity and yield stress were 1057 cP and 3.65 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.93 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was dried and milled as in Example 1.
  • the powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, with 20% CMC added simultaneously, and the composition was then mixed with a Silverson mixer at 8000 rpm for 5 min.
  • the product viscosity and yield stress were 377 cP and 1.06 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.93 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194- ppm of protease.
  • the press cake was dried and milled as in Example 1.
  • the powdered tormulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, and the composition was then mixed with a Silverson mixer at 8000 rpm for 5 min.
  • the product viscosity and yield stress were 432 cP and 1.39 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.93 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 194 ppm of protease.
  • the press cake was dried and milled as in
  • Example 1 The powdered formulation was then introduced into a STW sample in an amount of about 0.36% by weight thereof, and the composition was then mixed with a Silverson mixer at 8000 rpm for 5 min.
  • the product viscosity and yield stress were 552 cP and 1.74 dynes/cm 2 , respectively.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.51 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a STW solution in an amount of about 0.2% by weight thereof, with 10% CMC added simultaneously, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosity at 6 rpm was 377 cP.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.6 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a deionized water solution, a STW solution and 0.25% CaCl 2 solution, respectively, in an amount of about 0.2% by weight thereof, with 10% by weight of CMC added simultaneously, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosities were 512 cP, 372 cP and 358 cP, in de-ionized water, STW and 0.25% CaCl 2 solution, respectively.
  • Example 14 Analogous to the test performed in Example 1, with this sample about 20 3.2 mm diameter nylon beads (exhibiting a density each of about 1.14 g/mL) were dropped into each of the solutions (in de-ionized water, STW or 0.25% CaCl 2 solution) and the solutions were left at room temperature for 24 hours. None of the beads settled down to the bottom of the beakers after the time period expired, thus indicating excellent long-term suspension properties.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.51 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a deionized water sample in an amount of about 0.2% by weight thereof, with 10% by weight of CMC added simultaneously, and the composition was then activated with a propeller mixer at 2500 rpm for 10 min.
  • the product viscosity was 185 cP.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.4 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • a portion of the treated MFC broth was mixed with a given amount of xanthan gum broth and pre-hydrated CMC solution
  • the powdered formulation was then introduced into a STW solution and 0.25% CaC12 solution in an amount of about 0.2% by weight thereof, respectively, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosities at 6 rpm were 343 cP and 334 cP in STW and 0.25% CaCl 2 solutions, respectively.
  • About 20 3.2 mm diameter nylon beads (1.14 g/mL) were dropped into each of the solutions (in STW or 0.25% CaCl 2 solution) and the solutions were left at room temperature for 24 hrs. None of the beads settled down to the bottom of the beakers after the 24-hour time period.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.6 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a STW solution and 0.25% CaC12 solution in an amount of about 0.2% by weight thereof, respectively, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosities at 6 rpm were 306 cP and 293cP in STW and 0.25% CaCl 2 solutions, respectively.
  • About 20 3.2 mm diameter nylon beads (1.14 g/mL) were dropped into each of the solutions (in STW or 0.25% CaCl 2 solution) and the solutions were left at room temperature for 24 hours. None of the beads settled down to the bottom of the beakers after the 24-hour time period.
  • Example 17 MFC was produced in a 1200 gal fermentor with final yield of 1.6 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a STW solution and 0.25% CaC12 solution in an amount of about 0.2% by weight thereof, respectively, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosities at 6 rpm were 206 cP and 202 cP in STW and 0.25% CaC12 solutions, respectively.
  • About 20 3.2 mm diameter nylon beads (1.14 g/mL) were dropped into each of the solutions (in STW or 0.25% CaCl 2 solution) and the solutions were left at room temperature for 24 hours. None of the beads settled down to the bottom of the beakers after the 24-hour time period.
  • MFC was produced in a 1200 gal fermentor with final yield of 1.54 wt%.
  • the broth was treated with 350 ppm of hypochlorite and subsequently treated with 70 ppm of lysozyme and 350 ppm of protease followed with another 350 ppm of hypochlorite.
  • the powdered formulation was then introduced into a de-ionized water solution in an amount of about 0.2% by weight thereof, with 10% CMC added simultaneously, and the composition was then activated with an extensional homogenizer at 1500 psi for 2 passes.
  • the product viscosity at 6 rpm was 214 cP. ⁇ ach sample exhibited excellent and highly desirable viscosity modification and yield stress results. In terms of bacterial cellulose products, such results have been heretofore unattainable with bacterial cellulose materials alone and/or with the low complexity methods followed herein.

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AU2006250004A AU2006250004B2 (en) 2005-05-23 2006-05-23 Bacterial cellulose-containing formulations and method of producing effective bacterial cellulose-containing formulations
CN200680022042.9A CN101203615B (zh) 2005-05-23 2006-05-23 含有细菌纤维素的制剂以及生产含有有效细菌纤维素的制剂的方法
CA002609677A CA2609677A1 (en) 2005-05-23 2006-05-23 Bacterial cellulose-containing formulations and method of producing effective bacterial cellulose-containing formulations
JP2008513669A JP2008541728A (ja) 2005-05-23 2006-05-23 バクテリアセルロース含有調合物及び有効なバクテリアセルロース含有調合物の製造方法
MX2007014697A MX2007014697A (es) 2005-05-23 2006-05-23 Formulaciones que contienen celulosa bacteriana y metodo para producir formulaciones efectivas que contienen celulosa bacteriana.
BRPI0613298-7A BRPI0613298B1 (pt) 2005-05-23 2006-05-23 Método para a produção de uma formulação contendo celulose bacteriana e formulação contendo celulose bacteriana
KR1020077029842A KR101234471B1 (ko) 2005-05-23 2006-05-23 박테리아 셀룰로오스-함유 제형 및 효과적인 박테리아셀룰로오스-함유 제형의 생산 방법
NO20076536A NO20076536L (no) 2005-05-23 2007-12-18 Bakterielle cellulose-inneholdende formuleringer og fremgangsmate for fremstilling av effektive bakterielle cellulose-inneholdende formuleringer

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CN101487033A (zh) * 2009-02-23 2009-07-22 天津科技大学 微生物发酵直接生物合成细菌纤维素异型产品
EP2136647A1 (en) * 2007-04-24 2009-12-30 FMC Corporation Co-precipitated carrageenan/xanthan gum compositions and processes for their preparation
EP2496675B1 (en) 2009-11-04 2017-09-27 Colgate-Palmolive Company Microfibrous cellulose and alkaline earth metal ion structured surfactant composition
CN114410709A (zh) * 2022-01-20 2022-04-29 上海即索实业有限公司 一种高强度细菌纤维素复合材料及其制备方法
WO2024121315A1 (en) 2022-12-07 2024-06-13 Cellugy Aps A re-dispersible bacterial cellulose powder

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KR101300625B1 (ko) * 2013-02-26 2013-08-27 농업회사법인 주식회사 자담 미생물 셀룰로오스 겔 제조방법
JP5616479B1 (ja) * 2013-04-19 2014-10-29 大江生醫股▲ふん▼有限公司TCICo.Ltd バイオセルロース膜の製造方法
TWI671406B (zh) 2014-01-23 2019-09-11 國立大學法人九州大學 維持未分化性之培養材料
KR102336328B1 (ko) * 2017-04-25 2021-12-08 (주)아모레퍼시픽 고체 원물이 포함된 바이오셀룰로오스, 이를 제조하기 위한 배지 조성물 및 이의 제조방법
RU2695665C1 (ru) * 2018-11-09 2019-07-25 Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) Способ получения целлюлозного загустителя для пластичной смазки
JP7267583B2 (ja) * 2019-03-27 2023-05-02 国立大学法人高知大学 イオン性ポリマーの製造方法
KR102192110B1 (ko) * 2019-07-23 2020-12-16 숙명여자대학교산학협력단 박테리아 셀룰로오스 섬유를 포함하는 바이오 가죽 소재 및 이의 제조방법
RU2754368C1 (ru) * 2021-03-10 2021-09-01 федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный технический университет им. И.И. Ползунова" (АлтГТУ) Способ очистки бактериальной целлюлозы

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Cited By (11)

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WO2008079693A1 (en) 2006-12-19 2008-07-03 Cp Kelco U.S. Inc. Cationic surfactant systems comprising microfibrous cellulose
EP2094826A1 (en) * 2006-12-19 2009-09-02 CP Kelco U.S., Inc. Cationic surfactant systems comprising microfibrous cellulose
EP2094826A4 (en) * 2006-12-19 2010-05-05 Cp Kelco Us Inc CATIONIC SURFACE SYSTEMS COMPRISING MICROFIBREUS CELLULOSE
EP2136647A1 (en) * 2007-04-24 2009-12-30 FMC Corporation Co-precipitated carrageenan/xanthan gum compositions and processes for their preparation
EP2136647A4 (en) * 2007-04-24 2012-06-27 Fmc Corp TOGETHER COMPLETED CARRAGEEN / XANTHAN RUBBER COMPOSITIONS AND MANUFACTURING METHOD THEREFOR
US8323718B2 (en) 2007-04-24 2012-12-04 Fmc Corporation Co-precipitated carrageenan/xanthan gum compositions and processes for their preparation
CN101487033A (zh) * 2009-02-23 2009-07-22 天津科技大学 微生物发酵直接生物合成细菌纤维素异型产品
EP2496675B1 (en) 2009-11-04 2017-09-27 Colgate-Palmolive Company Microfibrous cellulose and alkaline earth metal ion structured surfactant composition
CN114410709A (zh) * 2022-01-20 2022-04-29 上海即索实业有限公司 一种高强度细菌纤维素复合材料及其制备方法
CN114410709B (zh) * 2022-01-20 2024-04-26 上海即索实业有限公司 一种高强度细菌纤维素复合材料及其制备方法
WO2024121315A1 (en) 2022-12-07 2024-06-13 Cellugy Aps A re-dispersible bacterial cellulose powder

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