US20150045543A1 - Isolation method for water insoluble components of a biomass and products provided therefrom - Google Patents

Isolation method for water insoluble components of a biomass and products provided therefrom Download PDF

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US20150045543A1
US20150045543A1 US14/454,972 US201414454972A US2015045543A1 US 20150045543 A1 US20150045543 A1 US 20150045543A1 US 201414454972 A US201414454972 A US 201414454972A US 2015045543 A1 US2015045543 A1 US 2015045543A1
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Prior art keywords
biomass
fractionated
subjecting
lignin
hemicellulose
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US14/454,972
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English (en)
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Melvin Mitchell
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GREEN EXTRACTION TECHNOLOGIES
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GREEN EXTRACTION TECHNOLOGIES
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Priority to US14/454,972 priority Critical patent/US20150045543A1/en
Priority to MX2016001905A priority patent/MX2016001905A/es
Priority to JP2016534771A priority patent/JP2016531744A/ja
Priority to EP14836435.9A priority patent/EP3033349A4/en
Priority to CA2921177A priority patent/CA2921177A1/en
Priority to PCT/US2014/050529 priority patent/WO2015023580A2/en
Priority to CN201480056139.6A priority patent/CN105849157A/zh
Priority to EP15830054.1A priority patent/EP3177768A1/en
Priority to CN201580002207.5A priority patent/CN105980630A/zh
Priority to EP15829162.5A priority patent/EP3180300A1/en
Priority to JP2017527187A priority patent/JP2017523811A/ja
Priority to JP2017527186A priority patent/JP2017526835A/ja
Priority to CN201580002208.XA priority patent/CN105793221A/zh
Priority to US14/619,451 priority patent/US20150247009A1/en
Priority to US14/619,406 priority patent/US20150152598A1/en
Priority to CA2919818A priority patent/CA2919818A1/en
Priority to CA2919784A priority patent/CA2919784A1/en
Priority to MX2016001908A priority patent/MX2016001908A/es
Priority to PCT/US2015/015368 priority patent/WO2016022172A1/en
Priority to MX2016001909A priority patent/MX2016001909A/es
Publication of US20150045543A1 publication Critical patent/US20150045543A1/en
Assigned to GREEN EXTRACTION TECHNOLOGIES reassignment GREEN EXTRACTION TECHNOLOGIES ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MITCHELL, MELVIN
Priority to US15/416,570 priority patent/US20170137578A1/en
Priority to US16/863,135 priority patent/US11174355B2/en
Priority to US17/494,167 priority patent/US20220025130A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • 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
    • C08B15/08—Fractionation of cellulose, e.g. separation of cellulose crystallites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/06—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/91—Polymers modified by chemical after-treatment
    • C08G63/912—Polymers modified by chemical after-treatment derived from hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00—Macromolecular compounds derived from lignocellulosic materials
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes
    • D21C3/224—Use of means other than pressure and temperature
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/62—Means for facilitating engagement or disengagement of coupling parts or for holding them in engagement
    • H01R13/627—Snap or like fastening
    • H01R13/6271—Latching means integral with the housing
    • H01R13/6272—Latching means integral with the housing comprising a single latching arm
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/62—Means for facilitating engagement or disengagement of coupling parts or for holding them in engagement
    • H01R13/627—Snap or like fastening
    • H01R13/6271—Latching means integral with the housing
    • H01R13/6273—Latching means integral with the housing comprising two latching arms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/648—Protective earth or shield arrangements on coupling devices, e.g. anti-static shielding  
    • H01R13/658—High frequency shielding arrangements, e.g. against EMI [Electro-Magnetic Interference] or EMP [Electro-Magnetic Pulse]
    • H01R13/6591—Specific features or arrangements of connection of shield to conductive members
    • H01R13/6594—Specific features or arrangements of connection of shield to conductive members the shield being mounted on a PCB and connected to conductive members
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R24/00—Two-part coupling devices, or either of their cooperating parts, characterised by their overall structure
    • H01R24/60—Contacts spaced along planar side wall transverse to longitudinal axis of engagement
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K5/00—Casings, cabinets or drawers for electric apparatus
    • H05K5/0026—Casings, cabinets or drawers for electric apparatus provided with connectors and printed circuit boards [PCB], e.g. automotive electronic control units
    • H05K5/0069—Casings, cabinets or drawers for electric apparatus provided with connectors and printed circuit boards [PCB], e.g. automotive electronic control units having connector relating features for connecting the connector pins with the PCB or for mounting the connector body with the housing

Definitions

  • the present invention relates to a process for isolating components of a biomass.
  • fractions and extractives provided in the process include the extraction, isolation, and purification of lignin, cellulose, sugars, hemicellulose, fibers and/or extractives.
  • biomass materials are comprised primarily of cellulose, hemicellulose and lignin, bound together in a complex and entangled gel-like structure along with amounts of extractables, pectins, proteins and/or ash.
  • successful commercial use of biomass as a chemical feedstock depends on the efficient and/or economical separation and isolation of these various constituents.
  • One step in the processing is the separation, or fractionation, of the biomass into its major components: extractives, hemicellulose, lignin, and cellulose.
  • extractives Many approaches have been investigated for disentangling the complex structure of the biomass. Once this separation has been achieved, a variety of paths are opened for further processing of each component into marketable products. For example, the possibility of producing products such as biofuels, polymers and latex replacements from biomass has recently received much attention. This attention is due to the availability of large amounts of cellulosic feedstock, the need to minimize burning or landfilling of waste cellulosic materials, and the usefulness of sugar and cellulose as raw materials substituting for oil-based products.
  • Lignin is a cross-linked racemic macromolecule with molecular masses in excess of 10,000 Da. It is relatively hydrophobic and aromatic in nature. The degree of polymerization in nature is difficult to measure, since it is often fragmented during typical extraction and the molecule consists of various types of substructures that appear to repeat in a haphazard manner. Different types of lignin have been described depending on the means of isolation. There are three monolignol monomers, methoxylated to various degrees: p-coumaryl alcohol, coniferyl alcohol, and sinapyl alcohol.
  • lignols are incorporated into lignin in the form of the phenylpropanoids p-hydroxyphenyl (H), guaiacyl (G), and syringyl (S), respectively.
  • Gymnosperms have a lignin that consists almost entirely of G with small quantities of H. That of dicotyledonous angiosperms is more often than not a mixture of G and S (with very little H), and monocotyledonous lignin is a mixture of all three. Many grasses have mostly G, while some palms have mainly S. All lignins contain small amounts of incomplete or modified monolignols, and other monomers are prominent in non-woody plants.
  • Cellulose is an organic compound with the formula (C 6 H 10 O 5 ) n , a polysaccharide consisting of a linear chain of several hundred to over ten thousand ⁇ (1 ⁇ 4) linked D-glucose units.
  • Cellulose is an important structural component of the primary cell wall of green plants, many forms of algae and the oomycetes.
  • Cellulose is an extremely abundant organic polymer on Earth. The cellulose content of cotton fiber is 90%, that of wood is 40-50% and that of dried hemp is approximately 45%.
  • Cellulose is mainly used to produce paperboard and paper. Smaller quantities are converted into a wide variety of derivative products such as cellophane and rayon.
  • the present invention provides a process for isolating various components of biomass that may be adapted to large-scale production, uses environmentally friendly solvents and/or is energy efficient. Moreover, the present invention provides a process for isolating various water insoluble components of the biomass in water soluble form while providing a biomass substantially devoid of hemicellulose, other sugars, and the water insoluble components.
  • the process includes pretreating the biomass with a first basic solution such as sodium hydroxide. Pretreatment may include mechanically altering the fibers to, for example, open up the fibers and to form a fluidized biomass.
  • the biomass with opened up fibers is then subjected to high frequency pulses and shear forces without denaturing the individual components of the biomass.
  • the biomass is then subjected to compressive force to separate a first liquid fraction from a first fractionated biomass.
  • the first fractionated biomass may again then be subjected to the same high frequency pulses and shear forces as previously, particularly if there are hemicellulose and/or sugars still present in the first fractionated biomass. Compressive forces are used to separate a second liquid fraction from a second fractionated biomass.
  • the second fractionated biomass is high in cellulose and water insoluble components including lignins and proteins, and is substantially devoid of hemicelluloses and sugars.
  • the second fractionated biomass is subjected to oxidation such as with hydrogen peroxide at a pH of 8 to 12.
  • the second fractioned biomass is then subjected to compressive forces to separate one or more water insoluble components of the biomass in water soluble and liquid form from a second fractionated biomass substantially devoid of hemicellulose, sugar and the water insoluble components of the biomass.
  • the present invention also provides a water insoluble component of a biomass in water soluble form at a pH of 5 to 12 at ambient temperature.
  • exemplary components which are typically water soluble include hemicellulose, sugars, pectins, some proteins and extractives.
  • Components which are typically water insoluble include lipids, lignins, some proteins and extractives.
  • FIG. 1 depicts a flow chart that outlines an embodiment of the process of the invention.
  • FIG. 2 depicts a flow chart that outlines another embodiment of the process of the invention.
  • the transitional phrase “consisting essentially of” (and grammatical variants) is to be interpreted as encompassing the recited materials or steps “and those that do not materially affect the basic and novel characteristic(s)” of the claimed invention. See, In re Herz, 537 F.2d 549, 551-52, 190 U.S.P.Q. 461, 463 (CCPA 1976) (emphasis in the original); see also MPEP ⁇ 2111.03. Thus, the term “consisting essentially of” as used herein should not be interpreted as equivalent to “comprising.”
  • a measurable value such as, for example, an amount or concentration and the like, is meant to encompass variations of ⁇ 20%, ⁇ 10%, ⁇ 5%, ⁇ 1%, ⁇ 0.5%, or even ⁇ 0.1% of the specified amount.
  • a range provided herein for a measureable value may include any other range and/or individual value therein.
  • biomass includes any non-fossilized, i.e., renewable, organic matter.
  • the various types of biomass may include plant biomass, animal biomass (any animal by-product, animal waste, etc.) and municipal waste biomass (residential and light commercial refuse with recyclables such as metal and glass removed).
  • Plant biomass or “ligno-cellulosic biomass” includes virtually any plant-derived organic matter (woody or non-woody) available for energy on a sustainable basis. “Plant-derived” necessarily includes both sexually reproductive plant parts involved in the production of seed (e.g., flower buds, flowers, fruit, nuts, and seeds) and vegetative parts (e.g., leaves, roots, leaf buds and stems). Plant biomass can include, but is not limited to, agricultural crop wastes and residues such as corn stover, wheat straw, rice straw, sugar cane bagasse and the like.
  • Plant biomass further includes, but is not limited to, woody energy crops, wood wastes and residues such as trees, softwood forest thinnings, barky wastes, sawdust, paper and pulp industry waste streams, wood fiber, herbal plant material brewing wastes, and the like. Additionally grass crops, such as switchgrass and the like have the potential to be produced in large-scale amounts and to provide a significant source of another plant biomass. For urban areas, potential plant biomass feedstock comprises yard waste (e.g., grass clippings, leaves, tree clippings, brush, etc.) and vegetable processing waste.
  • yard waste e.g., grass clippings, leaves, tree clippings, brush, etc.
  • the biomass comprises three basic chemical components/fractions, namely hemicellulose, cellulose, and lignins.
  • the biomass may also include lesser amounts of proteins, extractives, pectins, and ash depending on the biomass.
  • hemicellulose is a polymer (matrix polysaccharide) comprising the pentose and hexose sugars xylon, glucuronoxylon, arabinoxylon, glucomannon, and xyloglucan.
  • the sugars are highly substituted with acetic acid, and because of its branched structure, hemicellulose is amorphous. Hemicellulose is also easy to cleave via hydrolysis.
  • cellulose is a linear polymer (polysaccharide) of glucose sugars bonded together by ⁇ -glycosidic linkages to form lengthy linear chains. Hydrogen bonding can occur between cellulose chains results in a rigid crystalline structure which is resistant to cleavage.
  • Lignin is a polymer of phenolic molecules and is hydrophobic. It provides structural integrity to plants, i.e., it is the glue that maintains the plant intact.
  • Typical ranges of hemicellulose, cellulose, and lignin in, for example, a plant biomass such as corn stover are:
  • Ambient temperature includes the temperature of the surroundings in which the process of the invention takes place. Ambient temperature may include, but is not limited to, “room temperature,” and any temperature within the range of 10 to 40° C. (50 to 104° F.).
  • Individual components of the biomass may include, but are not limited to, lignin, cellulose, hemicellulose, proteins, pharmaceuticals, nutraceuticals and other materials obtained from the leaves, stems, flowers, buds, roots, tubers, seeds, nuts, fruit and the like of a plant.
  • Alcohol includes, but is not limited to, methanol, ethanol, isopropanol, propanol, isobutanol, butanol, and glycol.
  • a “short chain alcohol” generally includes C 1 to C 4 alcohols.
  • Water includes, but is not limited to, deionized water, spring water, distilled water, mineral water, tap water and well water, and mixtures thereof. “Water soluble” includes a component that can be dissolved in water or other solvent at ambient temperature. “Water insoluble” includes a component that cannot be dissolved in water or other solvent at ambient temperature.
  • a pretreatment step 90 may be conducted optionally at ambient temperature.
  • the biomass may be subjected to a pre-soak step 100 and/or disassembly step 110 .
  • the pre-soak step 100 may include contacting with a solvent with or without additives to facilitate the separation of the individual components.
  • the disassembly step 110 may include mechanical disassembling of the biomass to provide the biomass in a fluidized or flowable state or condition.
  • the biomass may be subjected to high frequency pulses and high shear forces to fractionate 120 or extract via, for example, the biomass fractionation apparatus and methods described in co-pending U.S. patent application Ser. No. 14/454,833, filed on Aug. 8, 2014 (Attorney Docket No. 1237-3) and co-pending U.S. patent application Ser. No. 14/454,952, filed on Aug. 8, 2014 (Attorney Docket No. 1237-2), the disclosures of which are incorporated by reference in their entireties.
  • Such fractionation does not denature the one or more individual components of the biomass.
  • Such fractionation provides a fraction or extracted product that can be separated from the fractionated or extracted biomass.
  • the fractionated or extracted biomass may be subjected to separation, namely filtration or screening 125 with or without agitation, followed by a compression force 130 , and then followed by additional filtration and/or separation with or without agitation 140 .
  • the fractions may be used to provide a desired product stream 150 .
  • the amount of hemicellulose and sugars in the fractionated biomass are monitored such as using a brix meter. If significant hemicellulose or sugars still are present the steps of subjecting to high frequency pulses and shear forces and subjecting to compressive forces are repeated.
  • the biomass in an initial pretreatment step 90 the biomass may be pre-soaked and contacted with a solvent such as with an alcohol, an aqueous alcohol, water or glycerin or co-solvent or mixture thereof in order to begin the fractionation or extraction of the biomass.
  • a solvent such as with an alcohol, an aqueous alcohol, water or glycerin or co-solvent or mixture thereof in order to begin the fractionation or extraction of the biomass.
  • the biomass may swell during this pretreatment step 90 .
  • the biomass may then be disassembled 110 such as by chopping, cutting, fraying, attrition or crushing prior to contact with the solvent 100 .
  • the biomass is, for example, fresh plant biomass or herbal plant material
  • the material may be contacted with alcohol.
  • the biomass is dried plant biomass or herbal plan material, it may be contacted with an aqueous alcoholic solution.
  • This aqueous alcoholic extraction may be performed in aqueous alcohol at different concentrations.
  • Suitable alcohols may be short chain alcohol, such as, but not limited to, methanol, ethanol, propanol, isopropanol, butanol and isobutanol.
  • the alcohol is ethanol.
  • the alcohol may be a co-solvent mixture such as a mixture of an alcohol and water.
  • the aqueous alcoholic solution may comprise from 0-100% (v/v) alcohol. More particularly, the aqueous alcoholic solution may comprise from 25-95% (v/v) alcohol. In a particular embodiment, the aqueous alcoholic solution is 25% (v/v) or more alcohol.
  • the aqueous alcohol may be 60% (v/v) alcohol. In another embodiment, the aqueous alcoholic solution may be 70% (v/v) alcohol. In yet another embodiment, the aqueous alcoholic solution may be 86% or more (v/v) alcohol.
  • the process for fractionating or extracting biomass may comprise contacting the biomass with glycerin or an aqueous glycerin solution. In yet another embodiment, the process for extracting biomass may comprise contacting the biomass with water.
  • the ratio of biomass/solids contacted with a solvent/liquids used may be 1:1 to 1:10 of solids to liquid. During contact with the solvent (alcohol or water) the fibers of the biomass may swell.
  • the fibers are opened up by chopping, cutting, fraying, attrition or crushing the biomass and are thereby provided in a fluidized or flowable form.
  • the biomass fibers may be processed in a mechanical high consistency fluidization machine such as a refiner or disk mill.
  • An exemplary disk mill is available from Sprout Waldron, Beloit or Andritz.
  • the biomass and particularly the fibrous material thereof may be altered without destroying the fibrous nature of the fibrous material so that the high frequency pulses and shear forces of the fractionation apparatus are accessible to the fibrous material.
  • the processing may take place for any amount of time necessary as would be understood by one of skill in the art as necessary to affect this step.
  • the disassembly process is performed for one minute or less.
  • the overall pretreatment step 90 may take place for any period of time that is sufficient for the fractionation or extraction process and may take place in any vessel, container or mixer suitable for contacting the biomass with a solvent and/or disassembling the fibers.
  • the pretreatment step may be any length of time between, for example, 15 minutes, 30 minutes or one hour, and 72 hours. In another embodiment, the pretreatment step may be 15 minutes or less.
  • the pretreatment step may be one minute or less.
  • the biomass in contact with the solvent may optionally be subjected to a compressive force, which can facilitate absorption of the solvent into the biomass.
  • the compression in the pretreatment step 90 may take place according to any technique that will be appreciated by one of skill in the art. In an embodiment of the invention, compression during the pretreatment step may be affected by a screw press.
  • the pretreatment may include the addition of an acid to prehydrolyze the biomass to facilitate removal of the hemicellulose.
  • Suitable acids for acidifying the pretreatment solution include inorganic acids such as nitric acid, hydrochloric acid and phosphoric acids, and organic acids, such as acetic acid or formic acid. If acidification/hydrolysis is desired, the pH of the solution will be about 0.5 to 7.0 and often may be between about 1.0 to 5.0.
  • a sequestering agent or chelating agent such as an aminocarboxylic acid or aminopolyphosphoric acid may also be used.
  • an anthraquinone may be utilized.
  • exemplary anthraquinones and derivatives thereof including 1-methylanthrazuinone, 2-methylanthraquinone, 2-ethylanthraquinone, 2-methoxyanthraquinone, 2,3-dimethylantraquinone, and 2,7-dimethylantraquinone.
  • an alkaline buffer such as an alkaline metal hydroxide, carbonate phosphate or boron may be included to facilitate separation of the hemicellulose and lignin individual components.
  • Suitable hydroxides include sodium hydroxide, sodium carbonate, and sodium borate. Mixtures or blends of the hydroxides may be used. If an alkaline metal hydroxide is added, the pH may be between about 7.0 to 13.0 and often may be between about 8.0 to 11.0.
  • the pretreatment step 90 may be conducted at ambient temperature, elevated temperature (30° C. to 90° C.) or using steam/vapor (greater than 100° C.). It is recognized that the vapor may be of the solvent.
  • the desire is to provide the fibers in a form wherein the components of the fibers can be readily fractionated using the high shear forces and pulses of the fractionation apparatus.
  • the selection of the conditions of the pretreatment step 90 such as solvent choice, temperature, pressure, time, additives, and the like will be dependent on the biomass and the components of that biomass to be fractionated and isolated, and will be within the skill of one in the art without undue experimentation.
  • the biomass is in fluid or flowable form may be subjected to fractionation 120 to fractionate or extract the biomass using shear forces and pulsation.
  • shear forces and pulsation are used in which the components of the biomass are not denatured or altered, and the chemical properties of the individual components are maintained wherein a portion of the fractions or extracts may be separated from the biomass.
  • the subjecting of the biomass to shear forces and high frequency pulses may take place for any amount of time necessary as would be appreciated by one of skill in the art as necessary to affect this step. In a particular embodiment, this step may takes place for one minute or less.
  • the fluidized biomass is rapidly accelerated from about 4 mph to about 120 mph under greater than 1000 pulses per second of energy while avoiding attrition of the biomass particles. This facilitates the ability of the cellular structure of the biomass to release its various fractions or constituents from the complex and entangled structure of the biomass without having the chemical properties and characteristics of the components being denatured.
  • the fractionated biomass material may then be subjected to a compression force 130 e.g., a crushing or macerating force optionally in the presence of additional solvent, wherein the compression force removes liquid fraction for collection while discharging a low liquid solids cake primarily being cellulose.
  • a compression force 130 e.g., a crushing or macerating force optionally in the presence of additional solvent, wherein the compression force removes liquid fraction for collection while discharging a low liquid solids cake primarily being cellulose.
  • the compression force may be applied according to any technique that is appreciated by one of skill in the art.
  • the compression force is affected by screws of a screw press that macerate the fractionated biomass.
  • the steps of subjecting to fractionation 120 and subjecting to fractionation can continue until the biomass fraction is substantially free of hemicellulose and sugars. This can be monitored or measured in a wide variety of matters including using a brix meter to measure sugar content, differential scanning calorimeter (DSC) to measure melt temperatures and differential thermal analysis (DTA) to measure area under melt curves.
  • DSC differential scanning calorimeter
  • DTA differential thermal analysis
  • the fractions or extracts provided according to the present invention may be further processed as outlined in FIG. 2 .
  • the fractions or extracts provided according to the present invention may be further processed as outlined in FIG. 2 .
  • the screened liquids e.g., liquid fractions
  • the screened liquids can be contacted with additional biomass, the biomass disassembled 210 , fractionated 220 , screened 240 , subjected to a compressive force 230 , and the solid fractionated biomass primarily being cellulosic and the liquid fractionated product stream separated 250 .
  • the fractionated biomass is high in cellulose can be used to make pulp and paper.
  • the biomass is subjected to oxidation at a pH above 7.
  • oxidation occurs by contacting the fractionated biomass with 0.1 to 1.5 percent hydrogen peroxide.
  • the hydrogen peroxide allows the lignin ether bond to cleave.
  • the phenolic groups in the lignin are ionized and the resulting radical is mainly of the phenoxyl radical type.
  • hydrogen peroxide is formed through dismutation of the superoxide anion.
  • the superoxide anion itself is not very reactive but the decomposition products of hydrogen peroxide include the very reactive hydroxyl radical.
  • the hydroxyl radical not only reacts with the lignin structures but also readily attacks the polysaccharides with subsequent glycosidic bond cleavage and the creation of new sites for peeling reactions. Once the perhydoxyl radical attaches to the lignin (or protein or water insoluble extractive) these individual components of the biomass become more polar and water soluble.
  • Other oxidation agents include alkali metal peroxides such as organic and inorganic peroxides including sodium peroxide, calcium peroxide, and magnesium peroxide. Moreover this reaction can be facilitated by inclusion of anthraquinone or its derivatives or other catalysts in the pretreatment step.
  • the centrifugation is used to provide a deant.
  • ultrafiltration or diafiltration membranes available from Millipore, Billerica, Mass.
  • a first membrane can be used to remove any remaining hemicellulose from the liquid fraction.
  • the first membrane is a 10K dalton screen.
  • the retentate will comprise the hemicellulose and the permeate will primarily comprise lignins, proteins, and extractives with a small amount of hemicellulose, sugars, and fiber fragments.
  • the second membrane will isolate the lignin, protein or extractive depending on the membrane as a retentate and any remaining hemicellulose, sugars, fragments, contaminants (e.g., heavy metals) as the permeate.
  • the second membrane is an 8K dalton screen. A further 3K dalton screen can be used to further isolate the desired component.
  • the cellulose and/or cellulose pulp provided by the fractionation and/or extraction process of the present invention can be used or applied in the preparation of paper and paper products.
  • paper products include, but are not limited to: paper; paperboard; and card stock.
  • Use of the paper products prepared from the cellulose and/or cellulose pulp provided by the present invention is not particularly limited.
  • the paper products can be produced with a wide variety of properties, depending on its intended use, which range from, for example: representing value, such as in paper money, bank notes, checks, security, vouchers and tickets; for storing information, such as in books and notebooks, scrapbooks, magazines, newspapers, art, letters; for personal use, such as in diaries, notes to oneself, etc.
  • the method by which the cellulose and/or cellulose pulp provided by the present invention is used in the production of paper and paper products is not particularly limited, and any method that would be appreciated by one of skill in the art may be used in the production of paper and paper products using the cellulose and/or cellulose pulp provided by the present invention.
  • the cellulose pulp provided according to the present invention can be fed to a paper machine where it is formed as a paper web and the water is removed from it by pressing and drying.
  • the cellulose pulp provided by the present invention may also be bleached to make the pulp whiter.
  • Typical chemicals and processes used in the bleaching of pulp include: chlorine; sodium hypochlorite; extraction with sodium hydroxide; oxygen; alkaline hydrogen peroxide; ozones; chelation to remove metals; enzyme treatment; peroxy acids; and sodium dithionite.
  • Typical chelation agents include, but are not limited to, EDTA and DTPA.
  • elemental chlorine free (ECF) and/or total chlorine free (TCF) methods of bleaching provide more environmentally friendly methods of bleaching.
  • ECF bleaching for example, prevents the formation of toxic chemicals such as dioxins.
  • An example of a TCF sequence for the bleaching of pulp is wherein the pulp would be treated with oxygen, then ozone, washed with sodium hydroxide then treated in sequence with alkaline peroxide and sodium dithionite.
  • the cellulose and/or cellulose pulp provided according to the present invention can be used or applied in the preparation and/or manufacture of paper coatings.
  • Cellulose and cellulose derivatives have been used to coat papers to enhance physical characteristics, for example, but not limited to, appearance, e.g., glossiness and finish, strength, rigidity and water resistance.
  • the manner in which the paper coatings prepared from the cellulose and/or cellulose pulp provided according to the present invention is not limited and the method used may be any that would be appreciated by one of skill in the art.
  • the cellulose and/or cellulose pulp provided according to the present invention can be used in the preparation of fibers.
  • fibers include, but are not limited to, regenerated cellulose fibers, for example, cellophane and rayon.
  • the cellulose and/or cellulose pulp provided according to the present invention can be used in consumables.
  • the type of consumable is not particularly limited, and applications can include, but are not limited to: microcrystalline cellulose or powdered cellulose used as inactive fillers in drug tablets; thickeners and/or stabilizers Powdered cellulose may also be used to improve characteristics of processed foods or foodstuffs, for example, to prevent caking and/or clumping of the processed food or foodstuffs within a container.
  • the cellulose and/or cellulose pulp provided according to the present invention can be used in scientific applications.
  • Cellulose is commonly used in the laboratory as the stationary phase for chromatography, in particular, thin layer chromatography.
  • Liquid and gel filtration typically use products prepared from cellulose, either alone or in combination with other filtration media, for example, diatomaceous earth.
  • the cellulose and/or cellulose pulp provided according to the present invention can be used in construction and building materials.
  • Cellulose insulation made from recycled paper is becoming popular as an environmentally preferable material for building insulation. It can be treated with boric acid as a fire retardant.
  • hydrogen bonding of cellulose in water can produce a sprayable, moldable material as an alternative to the use of plastics and resins.
  • the recyclable material can be made water and/or flame-resistant or fire retardant, and can provide sufficient strength for use as a building material.
  • the cellulose can be treated with cellulose enzymes to hydrolyze the crystalline cellulose to glucose followed by fermentation of the glucose with yeast or suitable microorganism to provide biofuel and/or bio feedstock. It is recognized that the hemicellulose and/or sugars previously separated from the fractionated biomass may be added back to be co-fermented with the cellulose.
  • fractionation or extraction according to the invention provides hemicelluloses and sugars.
  • Sugars and/or hemicelluloses provided by the process according to the invention may further be used in the preparation of biofuels such as, but not limited to, ethanol or the preparation of polymers/plastics.
  • biofuels such as, but not limited to, ethanol or the preparation of polymers/plastics.
  • the polymer is polylactic acid (PLA).
  • the lignin may be further separated and emulsified for further processing. Because the lignin has not been subjected to high temperatures, its functional groups have not chemically reacted and the isolated lignin may be more reactive.
  • the fraction or extract isolated and used is lignin.
  • lignin examples include, but are not limited to, for example: cement and concrete; animal feed pellets; animal feed molasses additives; road binder/dust control; pesticides; oil well drilling muds; adhesives; resins and binders; wallboard; dispersants; emulsifiers and wetting agents; agglomerants; chelants; leather treatment; anti-bacterial activity; lead acid batteries; oil recovery; water treatment; industrial cleaners; emulsion stabilizers; carbon black; inks and azo pigments; dyestuffs; micronutrients; fertilizers; refractories and ceramic brick additives; ore processing; and kitty litter.
  • the fraction or extract used is pulp, cellulose and/or cellulose pulp.
  • the applications and uses and applications of cellulose and/or cellulose pulp provided by the present invention include, but are not limited to, for example: paper and paper products; paper coatings; fibers; consumables; science; biofuels; building materials; insulation adhesives; and binders.
  • the lignin provided according to the present invention may comprise derivatives of lignin or lignin derivatives, for example, lignosulfonates or lignin amine.
  • the lignin provided by the present invention is used as a binder.
  • Lignin or lignin derivatives can be used as an adhesive, serving as a binding agent in pellets or compressed materials.
  • Lignin or lignin derivatives can be used in dust control, for example, on unpaved roads to reduce environmental concerns from airborne dust particles and stabilize the road surface.
  • lignin useful as a component in, for example: biodegradable plastic; coal briquettes; plywood and particle board; ceramics; animal feed pellets; carbon black; fiberglass insulation; fertilizers and herbicides; linoleum paste; dust suppressants; and soil stabilizers.
  • the lignin provided by the present invention is used as a dispersant.
  • Lignin or lignin derivatives can prevent the clumping and settling of undissolved particles in suspensions.
  • Lignin or lignin derivatives can prevent particles in suspension from being attracted to other particles and can reduce the amount of water needed to use a product comprising said particles in suspension.
  • the ability of lignin or lignin derivatives to act as a dispersant make lignin useful as a component in, for example: cement mixes; leather tanning; clay and ceramics; concrete admixtures; dyes and pigments; oil drilling muds; and pesticides and insecticides.
  • the lignin provided according to the present invention is used as an emulsifier.
  • Lignin or lignin derivatives may stabilize emulsions of immiscible liquids, for example, oil and water, making them highly resistant to separating.
  • the ability of lignin, lignosulfates and lignin amine to act as an emulsifier makes lignin or lignin derivatives a useful component in, for example: asphalt emulsions; pesticides; pigment and dyes; and wax emulsions.
  • lignin provided according to the present invention is used as a sequestrant.
  • Lignin or lignin derivatives can interact with metal ions, preventing them from reacting with other compounds and becoming insoluble.
  • Metal ions sequestered with lignin or lignin derivatives stay dissolved in solution, rendering them available to plants and preventing scaly deposits in water systems.
  • the ability of lignin and lignin derivatives to act as a sequestrant makes lignin a useful component in, for example: micronutrient systems; cleaning compounds; and water treatments for boilers and cooling systems.
  • lignin provided by the present invention can be used in concrete.
  • Lignin or lignin derivatives can aid in, for example: high performance concrete strength; concrete grinding; reducing damage caused by moisture and acid rain; and retarding cement composition setting.
  • lignosulfonates can contribute higher adsorption properties and zeta potential to cement particles and provide better dispersion characteristics to the cement matrix. Lignins can also improve the compressive strength of cement pastes.
  • lignin provided by the present invention can be used as an antioxidant.
  • Lignin can act as a free radical scavenger, and provide thermal protection to, for example, styrene polymers, butadiene polymers, rubber polymers, rubber, polypropylene and polycaprolactam.
  • the natural antioxidant properties of lignin make it useful in cosmetic and topical formulations, and lignosulfonates have been used in cosmetic compositions, such as makeup for decorative use and/or correction on skin.
  • lignin provided by the present invention can be used in asphalt.
  • uses include crack filling compositions for asphalt, enhancing water stability of asphalt, emulsifying agents for asphalt and fluidity modifiers that decrease production costs of asphalts.
  • lignin provided by the present invention may be applied to and/or used in or with carbon or graphite fibers, carbon fiber reinforced polymers and carbon nanotubes.
  • lignin provided by the present invention may be applied and used in the production of fiberboards, particleboards, wood fiber insulation boards, strawboards, oriented strand boards and the like as part of a binder composition.
  • a lignin may be added to a resin to provide a binder with reasonable wet strength.
  • the resulting board binder may then be used for panel boards, for example, in plywoods, hard boards, fiberboards or particle boards.
  • lignin provided by the present invention may be applied and used in foams, plastics and/or polymers.
  • polyurethanes comprising lignins can have improved flame resistance and/or fire retardance.
  • Epoxy resins can comprise a curing agent that comprises a lignin and/or a lignin derivative, such as a lignin-derived acetic anhydride.
  • Lignins for example S-free lignin, can be used in epoxy resins for fabricating printed circuit boards, or in products, such as automotive brakes.
  • Lignins may be added to polymers, for example, polyphenylene oxide-based polymers, to enhance modulus of elasticity, tensile strength and elongation at break values of the polymer.
  • Lignin can also act as a water absorption inhibitor and/or as a fluidization agent to facilitate polymer, for example, polyamide, processing, such as by injection molding, blow molding, extrusion or blow extrusion, to fabricate articles when mixed in solid or melt form.
  • Lignins for example, alkali lignin poly(propylene carbonate), can also be used to improve the thermal stability and mechanical properties of polymers.
  • lignin provided by the present invention may be applied and used in dust control.
  • lignin and glycerin in water can be applied to areas in which dust is a problem, such as, for example, in coal mines, transportation of coal, railways, roads, stock yards and the like.
  • Lignin for example, particular calcium lignin sulfonate powders, have been shown to stabilize contamination following a nuclear accident. Dust movement can also be controlled on a road surface by spraying with an emulsion comprising asphalt, lignosulfonate and water.
  • lignin provided by the present invention may be applied and used in papers as a sizing agent, to enhance paper tensile strength, and/or as a packaging laminate.
  • lignin provided by the present invention may be applied and used to provide chemicals through depolymerization of lignin.
  • Depolymeriziation of lignin can provide, for example, phenols, cresols, catechols, resorcinols, quinolines, vanillin, guaiacols and the like.
  • lignin provided by the present invention may be applied and used in batteries and to enhance the performance of energy storage devices.
  • graphite powder in batteries comprising a thin layer of lignin can be used to prevent the graphite powder from decreasing H overvoltage, while not affecting the condition of the graphite powder.
  • Lignin can also be used to protect negative plates of batteries from the formation of a passivating lead sulfate layer thereon.
  • lignin provided by the present invention may be applied and used as a fuel additive, or can be catalytically converted to gasoline/diesel by a combination of pyrolysis, thermal cracking, hydrocracking, catalytic cracking or hydrotreatment.
  • Lignin may further be used in catalytic hydrothermal gasification to provide fuel gas.
  • Lignin may also be used to wood pellets to produce better quality pellets with higher fuel value, or in artificial fire logs to provide improved flame properties.
  • lignin provided by the present invention may be applied and used as an additive to improve the characteristics of lubricants.
  • lignosulfonates can be used as a thickening agent for lubricating greases.
  • Greases can comprise lignin compositions to provide improved corrosion protection properties of the grease.
  • greases comprising lignin for example, hydrolytic lignin, can provide greater wear resistance to devices using the same.
  • Greases comprising lignin, such as lignosulfonate can improve the antifriction properties of the grease, and provide longer lubrication life for the grease.
  • lignin provided by the present invention may be applied and used in the production of latex and/or rubber.
  • lignin can be added to latex and/or rubber and function as a filler, pigment, modifier, extender or reinforcement for the same.
  • Lignin added to latex can increase oil resistance and/or tensile strength of rubber latex films. Rubbers reinforced with lignin can exhibit improved ozone resistance compared to rubbers without lignin added.
  • the method by which the lignin provided by the present invention is incorporated into latex and/or rubber is not particularly limited, and may be carried out by in any manner that will be appreciated by one of skill in the art.
  • the isolated proteins may be further isolated and hydrolyzed to single amino acids, peptides, and/or polypeptides.
  • Isolated protein may be used as a food supplement for humans and animals.
  • the protein content can be measured using Kjeldehl analysis.
  • the solid fraction is pretreated with NaOH sufficient to raise the pH of the cellulosic water slurry from about 4-7 to 10-12.
  • This basic mixture is allowed to age from a few seconds to 1 hour and again processed through the system starting at the disk mill which is subjected to water or steam injection in the mill for a few seconds to mechanically disassemble the cellulosic structure.
  • the fluidized wheat grass is then subjected to high shear forces for 1.5 to 3 seconds with pulses of 1824 to 912 times without denaturing the components of the wheat straw.
  • the combined mixture is subjected to compressive forces to separate the stream into liquid and a 20-60% cellulosic solids fractions.
  • the liquid fraction containing hemicellulose is added to the first and second fraction and undergoes further processing.
  • the solid fraction is treated with an oxidation agenti hydrogen peroxide, sufficient to raise the pH of the cellulosic water slurry from about 10-12 to 8-10.
  • This basic mixture is allowed to age from a few seconds to 1 hour and again processed through the system starting at the disk mill which is subjected to water or steam injection in the mill for a few seconds to mechanically disassemble the cellulosic structure.
  • the fluidized wheat grass is then again subjected to high shear forces for 1.5 to 3 seconds with pulses of 1824 to 912 times without denaturing the components of the wheat straw.
  • the combined mixture is screened and subjected to compressive forces to separate the stream into liquid and a 20-60% cellulosic solids fractions.
  • the liquid fraction containing lignin is retained.
  • the solid fraction is then treated again to raise the pH and the liquid fraction containing hemicellulose is added to the first and second fraction and undergoes further processing.
  • the solid fraction is then treated with an oxidation agent and rerun through the fractionation unit.
  • the liquid fraction containing lignin is added to the first liquid lignin fraction and further separated using a membrane.
US14/454,972 2013-08-12 2014-08-08 Isolation method for water insoluble components of a biomass and products provided therefrom Abandoned US20150045543A1 (en)

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US14/454,972 US20150045543A1 (en) 2013-08-12 2014-08-08 Isolation method for water insoluble components of a biomass and products provided therefrom
MX2016001905A MX2016001905A (es) 2013-08-12 2014-08-11 Metodo de aislamiento de componentes insolubles en agua de una biomasa y productos proporcionados de la misma.
JP2016534771A JP2016531744A (ja) 2013-08-12 2014-08-11 バイオマスの不水溶性成分のための単離方法およびそこから得られる産物
EP14836435.9A EP3033349A4 (en) 2013-08-12 2014-08-11 Isolation method for water insoluble components of a biomass and products provided therefrom
CA2921177A CA2921177A1 (en) 2013-08-12 2014-08-11 Isolation method for water insoluble components of a biomass and products provided therefrom
PCT/US2014/050529 WO2015023580A2 (en) 2013-08-12 2014-08-11 Isolation method for water insoluble components of a biomass and products provided therefrom
CN201480056139.6A CN105849157A (zh) 2013-08-12 2014-08-11 用于生物质的水不溶性组分的离析方法和由其提供的产品
JP2017527186A JP2017526835A (ja) 2013-08-12 2015-02-11 バイオマスからセルロースを単離するための方法およびそれから得られる産物
CA2919784A CA2919784A1 (en) 2013-08-12 2015-02-11 Method for isolating lignin from a biomass and products provided therefrom
EP15829162.5A EP3180300A1 (en) 2013-08-12 2015-02-11 Method for isolating lignin from a biomass and products provided therefrom
JP2017527187A JP2017523811A (ja) 2013-08-12 2015-02-11 バイオマスからリグニンを単離するための方法およびそれから得られる産物
EP15830054.1A EP3177768A1 (en) 2014-08-08 2015-02-11 Method for isolating cellulose from a biomass and products provided therefrom
CN201580002208.XA CN105793221A (zh) 2013-08-12 2015-02-11 用于从生物质中离析木质素的方法和由其提供的产品
US14/619,451 US20150247009A1 (en) 2013-08-12 2015-02-11 Method for isolating lignin from a biomass and products provided therefrom
US14/619,406 US20150152598A1 (en) 2013-08-12 2015-02-11 Method for isolating cellulose from a biomass and products provided therefrom
CA2919818A CA2919818A1 (en) 2013-08-12 2015-02-11 Method for isolating cellulose from a biomass and products provided therefrom
CN201580002207.5A CN105980630A (zh) 2014-08-08 2015-02-11 用于从生物质中离析纤维素的方法和由该方法提供的产品
MX2016001908A MX2016001908A (es) 2013-08-12 2015-02-11 Metodo para aislar celulosa de una biomasa y productos proporcionados de la misma.
PCT/US2015/015368 WO2016022172A1 (en) 2013-08-12 2015-02-11 Method for isolating cellulose from a biomass and products provided therefrom
MX2016001909A MX2016001909A (es) 2013-08-12 2015-02-11 Metodo para aislar lignina de un biomasa y productos proporcionados de la misma.
US15/416,570 US20170137578A1 (en) 2013-08-12 2017-01-26 Isolation method for water insoluble components of a biomass
US16/863,135 US11174355B2 (en) 2013-08-12 2020-04-30 Isolation method for water insoluble components of a biomass
US17/494,167 US20220025130A1 (en) 2013-08-12 2021-10-05 Isolation method for water insoluble lignin components of a biomass

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