CN105980630A - Method for isolating cellulose from a biomass and products provided therefrom - Google Patents
Method for isolating cellulose from a biomass and products provided therefrom Download PDFInfo
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- CN105980630A CN105980630A CN201580002207.5A CN201580002207A CN105980630A CN 105980630 A CN105980630 A CN 105980630A CN 201580002207 A CN201580002207 A CN 201580002207A CN 105980630 A CN105980630 A CN 105980630A
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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
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
-
- 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
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- 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
Abstract
A pretreated biomass is subjected to high frequency pulses and shear forces without denaturing and/or degrading 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 subjected to oxidation. The second fractioned biomass is then subjected to compressive forces to separate out one or more water insoluble components of the biomass in water soluble form and to provide cellulose that has not been denatured and/or degraded and has a lignin contact of less than 7 percent.
Description
Cross-Reference to Related Applications
The application is the part continuation application of U.S. Application No. 14/454,972 submitted on August 8th, 2014, this application claims in
On August 12nd, 2013 submit to U.S. Provisional Patent Application Serial No. 61/864,853, on November 27th, 2013 submit to U.S.
State's temporary patent application serial number 61/909,418 and the U.S. Provisional Patent Application Serial No. submitted in December in 2013 20
The priority of 61/919,194, the disclosure of above-mentioned patent application is herein incorporated by reference in its entirety by quoting.
Invention field
The method that the present invention relates to component for isolating biomass.The fraction provided in the method and the example bag of abstract
Include the extraction of lignin, cellulose, sugar, hemicellulose, fiber and/or abstract, isolation and purification.
Background of invention
Typically natural cellulosic material is referred to as " biomass ".The most eurypalynous biomass, including timber, paper, agricultural residual
Slag, herbaceous crops and lignocellulose city and industrial solid castoff have been considered as the life for broad range of commodity
Produce and the raw material of preparation.Plant biological material mainly comprises cellulose, hemicellulose and lignin, extracts with substantial amounts of
In the gel-like structure that thing, pectin, protein and/or ash are combined in complexity together and tangle.Therefore, biomass are as chemistry
The successful commercial use of raw material depends on the effective of these various compositions and/or is economically separated and isolates.
Biomass production, gather in the crops, store, transport and process in it is frequently necessary to a lot of step, to produce useful product
Product.One step of work in-process is biomass to be separated or are classified into its key component: abstract, hemicellulose, lignin
And cellulose, with small amount of pectin, ash, protein and cutin.Have studied a lot of method to untie answering of biomass
Miscellaneous structure.Once realize this separation, then open for each component is further processed into the various of vendible product
Approach.Such as, recently from biomass produce product such as bio-fuel, polymer and latex succedaneum probability be subject to
A lot of concerns.This concern is owing to the utilizability of a large amount of cellulosic materials, the burning making waste cellulosic materials or landfill
Minimize needs and the sugared and raw-material serviceability of cellulose alternatively oil-based products.
The component of one its isolation interesting of biomass is cellulose.Cellulose, particularly removes wooden fiber
Element be paper industry and bio-fuel production in institute of special interest.Cellulose is to have formula (C6H10O5) the organising of n
Compound, by hundreds of polysaccharide formed to the straight chain of the D-Glucose unit connected more than 10,000 β (1 → 4).Cellulose is green
The important structural constituent of the primary cell wall of plant, the algae of a lot of form and oomycetes.Cellulose is the abundantest on the earth
Organic polymer.The content of cellulose of cotton fiber is 90%, and the content of cellulose of timber is 40-50%, and dry big harl
Cellulose content is close to 45%.Cellulose is mainly for the production of cardboard and paper.Less amount changes into various derived product, example
Such as cellophane and artificial silk.If cellulose owing to exacting terms such as high temperature, high pressure, Chemical exposure, peracidity condition and/
Or high alkalinity condition degeneration and/or degraded, then use cellulose to be probably debatable as raw material.
Therefore, the needs of the sustainable existence system and method for improving, described system and method is used for providing cellulose
With substantially free from lignin, hemicellulose, other sugar and cellulose of ash, and consider such as environment and the energy worry, effect
Rate and the factor of cost effectiveness, limit degeneration and/or the degraded of cellulose components simultaneously.
Summary of the invention
It should be recognized that provide the concept that this general introduction selects to take reduced form introduction, further describe institute in the following discussion
State concept.This general introduction is not intended to identify key feature or the substitutive characteristics of the disclosure, is also not intended to limit the scope of the present invention.
The method that the present invention is provided to isolate cellulose, described method is adaptable to large-scale production, uses environment friend
Good solvent and/or be energy-conservation.Additionally, the present invention is provided to isolate cellulose and make cellulose go wooden method, its
Middle cellulose substantially free from lignin, hemicellulose, other other water-msoluble ingredients sugared and various, maintain simultaneously its structure with
Its structure in biomass is substantially similar.
Described method includes making biomass stand condition to isolate fine with the form of non denatured or non-degradable from biomass
Dimension element, and make cellulose stand oxidation, to remove the hemicellulose of any residual, lignin etc. with purifying cellulose level subsequently
Point.Described method includes biomass are carried out pretreatment, such as to remove most hemi-cellulose components.Pretreatment can include
Mechanical alteration fiber, such as to open fiber and to form fluidised biomass.Make the biomass with the fiber opened subsequently
Stand high-frequency impulse and shearing force, and do not make the individual components degeneration of biomass.Biomass are made to stand compression stress subsequently, to incite somebody to action
First liquid fraction separates with the first classification biomass.The first classification biomass can be made subsequently to be again subjected to height as before
Frequently pulse and shearing force, if particularly having hemicellulose and/or sugar to still exist in the first classification biomass.Compression stress
For the second liquid fraction is separated with the second classification biomass.The cellulose of the second classification biomass and water-msoluble ingredients bag
The content including lignin and protein is high, and substantially free from hemicellulose and sugar.The second classification biomass are made to stand oxidation.Subsequently
The second classification biomass are made to stand compression stress, to go out biology with the isolated in form of water solublity and liquid from the second classification biomass
The one or more of water-msoluble ingredients of matter, the content of the cellulose of described second classification biomass is high, and substantially free from half
The water-msoluble ingredients of cellulose, sugar and biomass, particularly lignin.
The cellulose of the second classification biomass is undenatured or degrades, i.e. itself and the fiber in the biomass before isolation
Element is substantially similar.It is believed that because present method avoids high temperature, high pressure, extreme electrochemical conditions, peracidity or alkalescence
Condition etc., therefore avoid and make cellulose degeneration and/or degraded, and provides the form taking to be particularly suitable as raw material
Remove wooden cellulose.
Accompanying drawing is sketched
Fig. 1 depicts flow chart, and it outlines the embodiment of the inventive method.
Fig. 2 depicts flow chart, and it outlines another embodiment of the inventive method.
Fig. 3 A and 3B depicts the various DSC carried out in the 3rd classification biomass of embodiment 2.
The detailed description of embodiment
In the following discussion, describe in detail embodiments of the present invention, enable to implement the present invention.Although with reference to this
A little specific embodiments describe the present invention, the present invention are embodied it will be appreciated that can take different form in,
And should not be construed as limited by the embodiment stated herein.On the contrary, it is provided that these embodiments so that the disclosure will be detailed and
Complete, and the scope of the present invention will be passed on completely to those skilled in the art.
The terminology used herein invented herein is only for describing the purpose of specific embodiment, and unawareness
The present invention to be limited.As used in the specification and claims of the present invention, singulative " one " (" a, "
" an ") and " described " (" the ") be also intended to include plural form, unless context clearly dictates otherwise.The present invention include as
Numerous substitute, amendment and equivalent is will become apparent from after consideration is described below.
It will be appreciated that although term " first, ", " second, ", " the 3rd, ", " a), ", " are b), " and " c), " wait in this article
Can be used for describing the various key elements of the present invention, but should be not limited by these terms.These terms are only used for the one of the present invention
Individual key element is distinguished with another key element.Therefore, the first element discussed below can be referred to as key element aspect, and similarly,
Three without departing from the teachings of the present invention.Therefore, term " first, ", " second, ", " the 3rd, ", " a), ", " b), " and " c), " etc.
It is not intended to necessarily order or other hierarchical structure be conveyed to relevant factor, and is used only as the purpose identified.Operation (or step)
Order be not limited to the order that presented in claims or figure, unless otherwise expressly stated.Step can be implemented simultaneously.
Unless otherwise defined, otherwise, all terms used herein (including technical term and scientific terminology) have and this
The identical meaning that the those of ordinary skill of field that the present invention belongs to is generally understood.It will be appreciated that term, such as conventional
Those defined in dictionary, it should be construed to have consistent with they meanings in the context and association area of the application
Meaning, and should not explain with the aspect of preferable or excessive form, unless so defined clearly herein.Invent herein
Terminology used herein be only used for describing the purpose of specific embodiment, and be not intended to limit the present invention.Carry herein
To all publications, patent application, patent and other is with reference to being incorporated by reference in its entirety by quoting.Situation in term conflict
Under, it is as the criterion with this specification.
Also as it is used herein, "and/or" refers to and includes one or more of any and institute of associated listed item
Possible combination, and when explaining with either-or ("or"), the shortage of combination.
Unless context it is further noted that otherwise, be clearly intended to can any combination to use each of invention described herein
Plant feature.Additionally, present invention further contemplates that in certain embodiments of the present invention, can get rid of or ignore any spy stated herein
Levy or the combination of feature.Illustrate, if description statement complex comprises component A, B and C, be clearly intended to negligible and do not want
Ask any one in protection A, B or C, or combinations thereof.
(and grammatical variants) be construed to include described material as used herein transition phrase " substantially by ... composition "
Or step " with the most substantially affect that of the basic of invention required for protection and novel characteristic (one or more of)
A bit ".See, about Herz, 537 F.2d 549,551-52,190 U.S.P.Q. 461,463 (CCPA 1976)
(being emphasis in original text source)；Referring further to MPEP § 2111.03.Therefore, term as used herein " substantially by ... composition "
Should not be construed as and be equal to " comprising ".
When mentioning measurable value such as, such as, when amount or concentration etc., as used herein term " about " means
Including defined amount ± 20%, ± 10%, ± 5%, ± 1%, ± 0.5% or the change of even ± 0.1%.Provided herein
The scope of measurable magnitude may be included in therein any other scope and/or individual values.
Term " biomass " includes the i.e. reproducible organic substance of any non-fossil.Various types of biomass can include
Plant biomass, animal organism matter (any animal byproduct (animal by-product), animal excrements etc.) and city are useless
Gurry biomass (remove the house of Recyclable such as metal and glass and light TRADE REFUSE).
Term " plant biomass " or " lignocellulose biomass " be actually comprised in continuable on the basis of, the energy
The organic substance (wooden or non-wood) of available any plant derivation." plant derivation " must include that participating in seed produces
Raw sexual reproduction plant part (such as bud, flower, fruit, pit and seed) and vegetalitas part (such as leaf, root, leaf bud and stem)
The two.Plant biomass may include but be not limited to agricultural crops garbage and residue, such as corn stalk, wheat straw, rice straw, bagasse
Etc..Plant biomass farther includes but is not limited to, wooden energy crop, timber waste and residue, such as tree, pin ebon
Forest thinning (forest thinning), bark garbage, sawdust, paper and pulp industry waste streams, the wood fiber, draft
Vegetable material brewages garbage etc..It addition, forage crop (grass crops), such as switchgrass (switchgrass) etc.
Deng, there are the potentiality with heavy production and the important sources providing another plant biomass.For urban area, potential
Plant biological raw material comprises garden garbage (such as the grass cuttings (grass clippings) pruned, leaf, the tree bits of pruning
(tree clippings), bushes etc.) and fruits and vegetables garbage.
Biomass comprise three kinds of basic chemical constituent/fraction, i.e. hemicellulose, cellulose and lignins.Depend on raw
Material, biomass may also include less amount of protein, abstract, pectin, cutin and ash.Specifically, hemicellulose is bag
Wooden containing pentose and hexose, glucuronic acid is wooden (glucuronoxylon), arabinose wooden (arabinoxylon), Portugal are sweet
Dew polysaccharide (glucomannon) and the polymer (matrix polysaccharide) of xyloglucan.Described sugar is replaced by acetic acid height, and because of it
Branched structure, hemicellulose is unbodied.Hemicellulose is also easy to decompose via hydrolysis.Under contrast, cellulose is Portugal
Grape sugar is bonded together the linear polymer (polysaccharide) to form the longest straight chain by β-glycosidic inkage.Hydrogen bonding can occur at fibre
Between dimension element chain, cause the rigid crystals structure of antidecomposition.Lignin is the polymer of phenol molecule, and is hydrophobic.It
Thering is provided structural intergrity for plant, i.e. it is the glue maintaining plant complete.
The typical scope of hemicellulose, cellulose and lignin in such as plant biomass such as corn stalk is:
| Component | Biomass dry weight |
| Cellulose | 30 - 50% |
| Hemicellulose | 20 -40% |
| Lignin | 10 -25% |
" ambient temperature " includes the temperature of the environment of the method generation of the present invention.Ambient temperature may include but be not limited to, " room
Temperature, " and any temperature in the range of about 0 to about 40 DEG C (30 to 104).
The individual components of biomass may include but be not limited to lignin, cellulose, hemicellulose, other sugar, protein, medicine
Thing (pharmaceuticals), nutrient (nutraceuticals), ash, pectin and cutin, and by the leaf of plant, stem,
Other material that flower, bud, root, tuber, seed, pit, fruit etc. obtain.
" alcohol " includes but not limited to methanol, ethanol, isopropanol, propanol, isobutanol, butanol and ethylene glycol." short chain alcohol " one
As include C1 to C4 alcohol.
" water " includes, but are not limited to deionized water, spring water, distilled water, mineral water, tap water and well water, and theirs is mixed
Compound." water miscible " includes may be dissolved in the component in water or other solvent at ambient temperature." water-insoluble " includes
The component in water or other solvent can not be dissolved at ambient temperature.
Referring now to Fig. 1, according to certain embodiments of the present invention, description is used for classification and the extraction of various biomass
Operation.Carry out pre-treatment step 90 the most at ambient temperature.Can make biomass stand pre-soak step 100 and/or
Decomposition step 110.Decomposition step 110 can include the machine decomposition of biomass, to provide fluidization or flowable state or condition
Under biomass.Pre-soak step 100 can include contacting with the solvent with or without additive, to promote individual components
Separation.In another embodiment, pre-treatment step can include hydrolysis (or in dry conditions biomass hydrolyze again) extremely
The humidity of about 20% to 50% increases.Hydrolysis can be realized by using steam treatment biomass.May then use that dividing of routine
From technology, such as, ultrafilter membrane or diafiltration membrane is used to make pretreated biomass stand separating step 105.In pre-treatment step 90
Afterwards, biomass can be made to stand high-frequency impulse and high shear force, with via, such as, on August 8th, 2014 submit to jointly treat
Examine U.S. Patent Application Serial Number 14/454,833 (attorney docket 1237-3) and on August 8th, 2014 submission co-pending
Biomass graded apparatus and method described in U.S. Patent Application Serial Number 14/454,952 (attorney docket 1237-2) are entered
Row classification 120 or extraction, above-mentioned patent application is incorporated by reference in its entirety by quoting.This type of classification does not make the one or more of biomass
Multiple individual components, the component of biomass, particularly cellulose degeneration and/or degraded.Cellulose is natively as raw with it
The form that the component of material is substantially the same.This type of classification provide can with the fraction that separate of biomass that is classified or that extract or
Extract product.Pulse (pulsation) and shearing force avoid changing the chemical characteristic of individual components, and are generally not resulted in this type of
The fragmentation of component.Can make classified or extract biomass stand separate, i.e. with or be not accompanied by stirring filtration or screening
125, it is followed by compression stress 130, and followed by being adjoint or being not accompanied by the other filtration of stirring and/or separate 140.Described
Fraction can be used for providing required product stream 150.In one embodiment, brix spindle is such as used to monitor through dividing
Hemicellulose in the biomass of level and the amount of sugar.If significantly hemicellulose or sugar still exist, repeatable stand high frequency arteries and veins
Punching and shearing force and the step standing compression stress.
As discussed briefly above, in initial pre-treatment step 90, can pre-preg biomass be allowed to connect with solvent
Touch, such as, contact with alcohol, aqueous alcohol (aqueous alcohol), water or glycerol or cosolvent or their mixture, with beginning
The classification of biomass or extraction, start to separate hemicellulose (hemicelloses) especially from biomass.Walk in this pretreatment
During rapid 90, biomass can expansion.Such as by contacting mincing, cut, wear and tear, rub or pressing before 100 with solvent
Broken, decomposable asymmetric choice net 110 biomass.In specific embodiment, if biomass are the freshest plant biomass or draft is planted
Thing material, then can make described material contact with alcohol.If biomass are dry plant biomass or herbaceous material, then can make its with
Aqueous alcohol solutions contacts.This hydrous alcohol extraction can be implemented in the aqueous alcohol of variable concentrations.Suitably alcohol can be short chain alcohol, such as
But it is not limited to methanol, ethanol, propanol, isopropanol, butanol and isobutanol.In specific embodiment, described alcohol is ethanol.Institute
State the mixture that alcohol can be cosolvent mixture, such as alcohol and water.Aqueous alcohol solutions can comprise the alcohol of 0-100% (v/v).More special
Not, aqueous alcohol solutions can comprise the alcohol of 25-95% (v/v).In specific embodiment, aqueous alcohol solutions is 25% (v/
Or more alcohol v).In another specific embodiment, aqueous alcohol can be the alcohol of 60% (v/v).In another embodiment,
Aqueous alcohol solutions can be the alcohol of 70% (v/v).In yet, aqueous alcohol solutions can be 86% or more (v/v)
Alcohol.In other embodiments, the method for classification or extraction biomass can include making biomass and glycerol or aqueous glycerol
Solution contacts.
In yet, the method being used for extracting biomass can include making biomass contact via with steam
Contact with water, to provide the humidity of 20% to 40% to increase.Typically, in other embodiments of the present invention, with used
The ratio of the biomass/solid of solvent/liquid contact can be the solid ratio liquid of 1:1 to 1:10.Connecing with solvent (alcohol or water)
Touching period, the fiber of biomass can expansion.
About decomposing fiber, first pass through and mince, cut, wear and tear, rub or crush biomass and open fiber, and therefore carry
For fluidization or the fiber of flowable form.Such as, can be in machinery high-consistency fluidisation machine such as refiner (refiner) or disc type
Processing biological fiber in mill (disk mill).Exemplary rim discharge mill available from Sprout Waldron,
Beloit or Andritz.By utilizing refiner or rim discharge mill, biomass and particularly its fibrous material can be changed,
And do not destroy the fibre property of fibrous material, so that the high-frequency impulse of grading plant and shearing force can be close to fibrous materials.
Described processing is sustainable as the skilled person will appreciate to be affected any required time quantum necessary to this step and occurs.
In specific embodiment, continue 1 minute or shorter enforcement decomposition method.
The sustainable any time section enough for classification or extracting method of total pre-treatment step 90 occurs, and can be in office
What vessel, container or be suitable to make biomass contact with solvent and/or generation in cellulolytic blender.At some embodiments
In, pre-treatment step can be between, the such as any duration between 15 minutes, 30 minutes or 1 hour and 72 hours.Real at another
Executing in mode, pre-treatment step can be 15 minutes or shorter.Pre-treatment step can be 1 minute or shorter.In pre-treatment step,
The biomass contacted with solvent can be made optionally to stand compression stress, and described compression stress can promote that solvent enters the suction in biomass
Receive.Compression in pre-treatment step 90 can occur according to any technology that it will be appreciated by persons skilled in the art that.The present invention's
In embodiment, the compression during pre-treatment step can be affected by fly press.
In another embodiment, pretreatment can include adding weak acid so that pre-hydrolysis of biomass, to promote hemicellulose
Removing.Suitable acid for acidizing pretreatment solution (solvent) includes mineral acid, such as nitric acid, hydrochloric acid and phosphoric acid, and has
Machine acid, such as acetic acid or formic acid.Recognize that weak acid is not likely to be required as the interpolation of acetic acid or formic acid, because natural amount is same
The acid of sample is present in biomass.If desired acidifying/hydrolysis, then the pH of solution would be about 0.5 to 7.0, and generally will be between about
Between 1.0 to 5.0.It is also possible to use screening agent (sequestering agent) or chelating agen (chelating agent) such as
Amino carboxylic acid or amino polyphosphoric acid.
Additionally, it may include help the compound of catalysis delignification.In one embodiment, available anthraquinone
(AQ).Exemplary anthraquinone and derivant thereof include 1-methylanthracene quinone, 2-methylanthraquinone, 2-ethyl-anthraquinone, 2-methoxy anthraquinone,
2,3-dimethyl anthraquinone and 2,7-dimethyl anthraquinone.
In another embodiment, it may include ealkaline buffer such as alkali metal hydroxide, carbonate, phosphate or boron
Hydrochlorate, to promote hemicellulose and the separation of lignin individual components.Suitably buffer agent can include sodium hydroxide, sodium carbonate and
Sodium tetraborate.Hydroxide, carbonate and boratory mixture or blend can be used.If interpolation alkali metal hydroxide,
Then pH between about 7.0 to about 13.0, and can may typically lie between about 8.0 to about 11.0.
Can at ambient temperature, raise temperature (20 ° of C to 90 ° of C) under or use steam/steam (more than 100 ° of C) enter
Row pre-treatment step 90, with hydration or rehydrated biomass.Recognize that steam can be the steam of solvent.
Isolation or the removing of hemicellulose can be realized in this stage.Available ultrafiltration or diafiltration provide and have biomass
The hemicellulose of 80% to 95% retain material, and comprise the penetrant of the biomass removing major part hemicellulose.Notice
Retaining material and can include the organic acid of isolation, such as acetic acid or formic acid, it can be removed from retaining material, and be used for as above institute
Biomass are carried out pretreatment with stating.Hemicellulose can be dried to avoid fermentation or mycete to produce, and be subsequently used as such as ethanol
The raw material produced.
Generally speaking, it is desirable to be to provide the fiber of following form: wherein use the high shear force of grading plant and the pulse can
Easily make the component classification of fiber, be removed with major part hemicellulose.The condition of pre-treatment step 90 such as solvent selects
Take, temperature, pressure, time, the selection of additive etc. will depend upon which biomass and that biomass of to be fractionated and isolation
Component, and by within the technical scope of those skilled in the art, and without excessive experiment.Extreme and harsh bar can be avoided
Part, in order to do not make cellulosic component degeneration and/or degraded.
After removing hemicellulose 105, the biomass of fluid or flowable form can be made to stand classification 120, to use
Shearing force and pulse carry out classification or extract biomass.Will be recognized by specific embodiment, unchanged in the component of biomass
Property or change use shearing force and pulse in the case of maintaining the chemical property of individual components, wherein can divide from biomass
Separate out a part of fraction or extract.Make biomass stand shearing force and high-frequency impulse is sustainable will anticipate such as those skilled in the art
Know any required time quantum necessary to this step that affects arrived to occur.In specific embodiment, this step sustainable 1
Minute or shorter generation.In operation, under the energy per second more than 1000 pulses, fluidised biomass are fast from about 4 mph
Speed accelerates to about 120 mph, avoids the friction of biological particles simultaneously.This facilitate the cellularity of biomass from biomass
Complicated and the structure tangled discharges its various fraction or the ability of composition, and do not make chemical property and the characteristic degeneration of component
Or degraded.
Classified biological material can be made subsequently optionally to stand compression stress 130 such as in the presence of other solvent, pressure
Broken power or macerate power (macerating force), wherein said compression stress removes liquid fraction and is used for collecting, discharges master simultaneously
If the solids cake compresses of the low liquid of cellulose.Compression stress can be applied according to any technology that skilled person be aware that.?
In specific embodiment, compression stress is affected by the screw rod of fly press, and described fly press is macerated classified
Biomass also can include optional stirring.
Stand classification step 120 and stand classification sustainable until biomass fraction generally without hemicellulose and
Sugar.This can take various means be monitored or measure, including use brix spindle measure sugar content, use poor
Show that scanning calorimeter (DSC) is measured melt temperature and uses differential thermal analysis (DTA) to measure the area under melting curve.
In one embodiment, the first classification biomass can be made to stand condition so that the pH of the first classification biomass improves
To about more than 9.Such as, biomass and weak caustic alkali can be made, such as 0.1 to 0.5% w/w sodium hydroxide contact based on water.
The fraction provided according to the present invention and extract can as Fig. 2 summarizes be provided further.The liquid of screening can be made
Body (such as liquid fraction) contacts with other biomass, described biomass through decompose 210, classification 220, screening 240, through by compression
Power 230, and the biomass of solid-state classification be mainly cellulose and separate liquid classification product stream 250.Although recognizing that solid-state is divided
Level solid is generally cellulose, but it still has the lignin and some hemicelluloses being attached on cellulosic molecule.
It is not intended to be limited to single theory, applicant believes that hemicellulose in a small amount allows lignin to be water miscible, and heavy
It is removed during shallow lake.
The most classified biomass generally without hemicellulose and sugar, then make biomass stand under the pH more than 7
Oxidation, it is noted that described classified biomass typically have the pH of about 7, and pH is about 9.In one embodiment,
Aoxidize to be contacted with about 0.1% to about 5% hydrogen peroxide by classified biomass and occur.Such as, about lignin remove, from
Analysis and purification, hydrogen peroxide allows the cracking of lignin ehter bond.Specifically, the phenolic group in lignin is ionized, and the base of gained
It is mainly phenoxy group type.Hydrogen peroxide is formed by the disproportionation of superoxide anion.Superoxide anion is originally
Body reactivity is not very strong, but the catabolite of hydrogen peroxide includes the strongest reactive hydroxyl.Hydroxyl not only with wood
Quality structural response, and easily attack polysaccharide, with glycosidic inkage decomposition subsequently and the product of the novel site for stripping reaction
Raw.Once hydroperoxyl (perhydoxyl) and lignin (or protein or water-insoluble abstract) combine, these biomass
Individual components become polarity and water solublity is higher.Other oxidant includes alkali-metal peroxide, the most organic and inorganic mistake
Oxide, including sodium peroxide, calper calcium peroxide, Magnesium dioxide and SODIUM PERCARBONATE.Additionally, can be by including in pre-treatment step
Anthraquinone or derivatives thereof or other catalyst promote this reaction.
In another embodiment, preparation oxidation mixture.Oxidation mixture is by by ealkaline buffer such as alkali metal
Hydroxide, carbonate, phosphate or borate, oxygen anion (oxyanions) source and short chain organic acid mix
To provide oxidation mixture to provide.Suitably ealkaline buffer includes sodium hydroxide, sodium carbonate and sodium tetraborate.Suitably oxygen
Source of anions includes hydrogen peroxide and organic and inorganic peroxide, such as sodium peroxide, calper calcium peroxide, Magnesium dioxide and mistake
Sodium carbonate.Optionally, can be by sulphuric acid or sodium sulfate (i.e. S2 -Or HS-The source of ion) as oxygen anion nucleophilic sulfide catalytic
Agent includes, to promote delignification.When using cellulose as raw material, esterification and the ester of its base catalysis the most also will be promoted
Exchange.In one embodiment, oxygen anion can be generated by ozonisation via the method for electricity.Suitably short chain organic acid can
Including acetic acid (vinegar) and formic acid.By alkali carbonate stabilizer such as sodium carbonate or sodium bicarbonate and Mn catalyst are mixed
Stable catalyst mixture is provided together.Exemplary Mn catalyst is the mangaic acid of chelating, such as manganese chelating amino acids
Thing.In one embodiment, stable catalyst mixture can be powder solid form.
Subsequently, such as by stable catalyst is mixed by the catalyst of powder type and the mixing of the second classification biomass
Compound is applied in the second classification biomass.Subsequently liquid oxidatively mixture is added in the second classification biomass, and carry out
Mixing, and allow oxidation to occur the most about 1 minute to about 48 hours.The second oxidized classification biomass are made to stand to have subsequently
The compression stress of optional spin, to provide the 3rd classification biomass of content of lignin low (i.e. generally less than about 4% to about 8%),
Threeth liquid fraction high with content of lignin.3rd classification biomass can be the most oxidized, and stands to have optionally
The compression stress of spin, to provide the 4th classification biomass of content of lignin the lowest (i.e. generally less than about 2% to about 4%)
Fourth liquid fraction significantly high with content of lignin.The isolation step of biomass and repeating with oxidation mixture contacts and subsequently
Compression can be repeated several times, until classified biomass have less than about 0 to about 2% lignin, last step (step or
More multistep) it is conventional water rinsing step.
After separation, can separate further, isolate and/or the present water miscible individual components of purification, such as lignin, described
The co-pending U.S. Application No. that separation, isolation and/or purification are such as submitted on February 11st, 2015(generation
Reason people's Reference Number 1237-4IP2) described in, the disclosure of which is herein incorporated by reference in its entirety by quoting.In one embodiment,
Centrifuging is used to provide decantate (decant).Subsequently, can use and such as be available from Millipore, Billerica,
The ultrafilter membrane of Massachusetts or diafiltration membrane.The first film can be used to remove any remaining hemicellulose from liquid fraction.
In one embodiment, the first film is 10K dalton's screen cloth.Retain material and will comprise hemicellulose, and penetrant will be main
Comprise lignin, protein and abstract, with hemicellulose, sugar and fibre debris in a small amount.Second film will depend upon which that film will
Lignin, protein or abstract isolate as retaining material, and by any remaining hemicellulose, sugar, fragment, pollutant
(such as heavy metal) isolates as penetrant.In one embodiment, the second film is 8K dalton's screen cloth.Another 3K dalton sieves
Net can be used for isolating required component further.Cellulose can be made to stand esterification or the ester exchange of base catalysis.
In specific embodiment, can by the cellulose provided by the classification of the present invention and/or extracting method and/or
Cellulose pulp is used in or applies in the preparation of paper and paper products.The example of paper products includes but not limited to: paper, cardboard and card
Sheet material (card stock).The purposes of the paper products prepared by the cellulose provided by the present invention and/or cellulose pulp
It is not particularly limited.Depending on its desired use, can produce the paper products with various character, described purposes contains, example
As: represent and be worth, such as in bank note, banknote (bank notes), check, bond, receipt and ticket；For storing information,
Such as in books and notebook, scrapbook, magazine, newspaper, the fine arts, letter；Day for private purposes, such as eat alone
In note, notes etc. and note；For exchanging, such as in the exchange between individual and/or crowd；For packaging and container, example
As cardboard, kraft liner, container cardboard, liner board, beverage and/or food containers, liquid container, Concha Arcae case, paper bag,
In envelope, packaging tissue paper, papyrus paper (Charta emporetica) and wallpaper；For cleaning, such as toilet paper, napkin,
In towel paper, facial tissue and cat litter；For building, such as paper mold, origami, paper helicopter, quilling, paper honeycomb, be used as multiple
In core material, paper skill engineering (paper engineering), drawing paper and paper clothing in condensation material；With other purposes, such as
In emery paper, sand paper, blotting paper, litmus paper, universal indicator paper, paper chromatography, electric insulation paper using (referring further to electrolyte
And dielectric constant) and filter paper.
Cellulose and/or cellulose pulp is provided to be used in the method in the production of paper and paper products not by spy by the present invention
Do not limit, and any method that it will be appreciated by persons skilled in the art that can be used on use the cellulose that provided by the present invention and/
Or in the production of the paper of cellulose pulp and paper products.Such as, the cellulose pulp provided according to the present invention can be fed to making
In paper machine, it is formed as paper web wherein, and removes water from which by pressing and being dried.Also can will be provided by the present invention
Cellulose pulp bleach, so that paper pulp is whiter.The typical chemicals being used in the bleaching of paper pulp and method include:
Chlorine, sodium hypochlorite, use sodium hydroxide extraction, oxygen, alkaline hydrogen peroxide, ozone, chelating are to remove metal, ferment treatment, peracid
And sodium dithionite.Typical chelating agen includes but not limited to EDTA and DTPA.Although being limited to the most especially pass through the present invention
The cellulose provided and/or the method for bleaching of cellulose pulp, but element-free chlorine (ECF) and/or float completely without chlorine (TCF)
White method provides more environmentally friendly method for bleaching.TCF bleaches, and such as, prevents the formation of toxic chemical such as two English.With
Example in the TCF order of association with pulp bleaching is that wherein paper pulp will process through oxygen, subsequently ozone, wash through sodium hydroxide, presses subsequently
Order processes through alkaline peroxide and sodium dithionite.
In other embodiments, the cellulose provided according to the present invention and/or cellulose pulp can be used in or apply
In the preparation and/or manufacture of paper coating.Cellulose and cellulose derivative has been used to be coated strengthening physics to paper
Characteristic, such as but not limited to, outward appearance, such as glossiness and surface smoothness (finish), intensity, rigidity and resistance to water.By basis
It is unrestricted that cellulose that the present invention provides and/or cellulose pulp prepare the mode that paper coating taked, and used
Method can be any one that it will be appreciated by persons skilled in the art that.
In other embodiments, the cellulose provided according to the present invention and/or cellulose pulp can be used on the system of fiber
In Bei.The example of fiber includes but not limited to the cellulose fibre of regeneration, such as cellophane and artificial silk.
In other embodiments, the cellulose and/or the cellulose pulp that provide according to the present invention can be used in consumable goods.
The type of consumable goods is not particularly limited, and application may include but be not limited to: as the crystallite of the inert filler in medicinal tablet
Cellulose or cellulose powder；Thickening agent and/or stabilizer.Cellulose powder can also be used for improving processed food or the spy of food
Property, such as, in order to prevent processed food or the food caking in container and/or gathering.
In other embodiments, the cellulose and/or the cellulose pulp that provide according to the present invention can be used on scientific application
In.Cellulose is used as the fixing phase of chromatography, particularly thin layer chromatography the most in the lab.Liquid and gel filtration typical case
Ground uses the product prepared by cellulose, or is used alone, or is applied in combination with other filter medium such as kieselguhr.System
Standby various filtrations can comprise the cellulose of the present invention.
In other embodiments, the cellulose provided according to the present invention and/or cellulose pulp can be used on construction and build
Build in material.Just become as the preferred material of environment for structural insulated material by reclaiming standby cellulose insulation material made of paper
Obtain popular.It can use the boric acid as fire retardant to process.Additionally, the hydrogen bonding that cellulose is in water can produce sprayable,
Moldable material, as plastics and the replacement of resin applications.Callable material can be made into water-fast and/or fire-resistant or fire-retardant
, and may function as the intensity that construction material provides enough.
In another embodiment, cellulose treatment cellulose can be used, so that crystalline cellulose is hydrolyzed into glucose,
It is then used by yeast or suitably microorganism makes glucose fermentation, to provide bio-fuel and/or biological raw material.Recognizing can be by
The hemicellulose and/or the sugar interpolation that separate from classification biomass are gone back, to ferment altogether with cellulose before.
In another specific embodiment, classification or extraction according to the present invention provide hemicellulose and sugar.By root
The sugar and/or the hemicellulose that there is provided according to the method for the present invention can be further used in the bio-fuel preparation such as but not limited to ethanol
In, or be used in the preparation of polymers/plastics.One such embodiment is that the fermentation of provided fraction is to produce second
Alcohol.In another embodiment, polymer is polylactic acid (PLA).In another embodiment, lignin can be through separating further
And emulsifying, for further processing.Because lignin does not stands high temperature, so its functional group does not carries out chemical reaction, and
The reactivity of the lignin separated can be higher.
There is provided following example that the present invention is described, and should not be construed as its restriction.
Embodiment
Embodiment 1
Wheat straw
The dry wheat straw (straw) of 10Kg is chopped into the handle of 2 inches long.Straw is simply rinsed, to remove sand with clean cold water
Son and dust.Wheat straw is made to stand in water or the steam injection entrance rim discharge mill of last for several seconds subsequently, fine with machine decomposition
Dimension element structure.Make fluidised wheat straw stand to continue the high shear force of 1.5 to 3 seconds subsequently, with 1824 to 912 subpulses, and
Do not make component degeneration and/or the degraded of wheat straw.The mixture making combination stands compression stress, with stream is separated into liquid and
20-60% cellulose solid-state fraction.Retain the liquid fraction containing hemicellulose.
Use NaOH solid-state fraction is carried out pretreatment, this NaOH be enough to the pH making cellulose water slurry from about 4-7 improve to
10-12.Allow this alkaline mixt ageing several seconds to 1 hour, and process again by the system originating in rim discharge mill,
Described mixture stands water or the steam injection of last for several seconds in mill, with machine decomposition cellulosic structure.Make subsequently
Fluidised wheat straw stands the high shear force continuing 1.5 to 3 seconds, adjoint 1824 to 912 subpulses, and does not make the component of wheat straw
Degeneration.The mixture making combination stands compression stress, so that stream to be separated into liquid and 20-60% cellulosic solid-state fraction.To contain
The liquid fraction of hemicellulose is added in the first and second fraction, and is subjected to further process.
Using oxidants hydrogen peroxide to process solid-state fraction, hydrogen peroxide be enough to the pH making cellulose water slurry from about 10-12
It is down to 8-10.Allow this alkaline mixt ageing several seconds to 1 hour, and again by originating at the system of rim discharge mill
Reason, described mixture stands water or the steam injection of last for several seconds in mill, with machine decomposition cellulosic structure.Subsequently
Make fluidised wheat straw stand to continue the high shear force of 1.5 to 3 seconds, with 1824 to 912 subpulses, and do not make the group of wheat straw
Divide degeneration.The mixture of combination is screened, and is subjected to compression stress, stream to be separated into liquid and 20-60% fiber
Element solid-state fraction.Retain the liquid fraction containing lignin.Process solid-state fraction is to raise pH the most again, and will be fine containing half
The liquid fraction of dimension element is added in the first and second fraction, and is subjected to further process.Use subsequently at oxidant
Reason solid-state fraction, and again run through stage unit.Liquid fraction containing lignin is added to the first liquid lignin
In fraction, and film is used to separate further.
Embodiment 2
By the dry switchgrass steam activation of 423 grams with rehydrated when the water of about 25% to 50% in single disk refiner, with
Switchgrass under fluidization or flowable state is provided.In switchgrass, naturally occurring carboxylic acid (acetic acid and formic acid) makes pH be down to 3
Below.Make the switchgrass through hydration/activation stand compression stress, with isolate the high liquid of hemicellulose level and cellulose and
The biomass that content of lignin is high.Make hemicellulose/liquid stand 1 to 5kD ultrafilter membrane subsequently, using by acetic acid and formic acid as oozing
Thing removes thoroughly, to re-use in the process.
Green Extraction Technology grading plant is used to make biomass stand high-frequency impulse and shearing subsequently
Power, and do not make lignin degeneration and/or degraded, the U.S. Application No. 14/454 that described device was submitted on August 8th, 2014,
Described in 833.Within the most about 15 to about 30 seconds under the pulse of 912 to 1824, carry out classification biomass, to provide the first classification biological
Matter and the first liquid fraction.The first classification biomass are made to contact, so that pH is raised to about 9 with 0.3% w:w sodium hydroxide based on water
Above.The first classification biomass are made to stand compression stress subsequently, will have the second liquid level of most of remaining hemicellulose
The second classification biomass high with cellulose and content of lignin are divided to separate.
The second classification biomass are made to stand oxidation, to be separated with cellulose by lignin subsequently.Form oxidation mixture, and
It comprises 2000ml and uses 60g sodium hydroxide and 3% hydrogen peroxide of 300ml acetate buffer.By by 2g sodium carbonate stabilizer and
15mg powder manganese amino-acid chelate catalyst is mixed to form catalyst/stabilizer blend.By powder catalyst/stable
Agent composition is applied in the second classification biomass, and makes it contact with liquid oxidatively mixture subsequently, and aoxidizes 60 minutes.Make
Make the second oxidized classification biomass stand compression stress with the Double helix forcing press with stirring, have less than 7% to provide
The 3rd classification biomass that the content of cellulose of content of lignin is high and high the 3rd liquid fraction of water-soluble lignin content.With
Rear use 1500 ml hydrogen peroxide and other component of same amount of oxidation mixture and catalyst/stabilizer blend make
Three classification biomass reoxidation 60 minutes.Make the 3rd oxidized classification biomass stand compression stress subsequently, have to provide
The 4th classification biomass that the content of cellulose of the content of lignin less than 7% is high and high the 4th liquid fraction of content of lignin.
Repeat whole oxidizing process subsequently, use 1000ml hydrogen peroxide oxidation 120 minutes, and be then subjected to compression stress, to provide tool
There are the 5th classification biomass that the content of cellulose of the content of lignin less than 5% is high.
Fig. 3 A and 3B provides the DSC of the 3rd classification biomass, it is noted that Fig. 3 B illustrates the existence owing to acetic acid,
Cellulose is acetylation.
Embodiment 3
By the dry wheat straw steam activation of 423 grams with rehydrated when the water of about 25 to 50% in single disk refiner, to provide
It is in the switchgrass under fluidization or flowable state.In wheat straw naturally occurring carboxylic acid (acetic acid and formic acid) make pH be down to 3 with
Under.The wheat straw making hydration/activation stands compression stress, contains isolating the high liquid of hemicellulose level and cellulose and lignin
Measure high biomass.Hemicellulose/liquid is made to stand 1 to 5kD ultrafilter membrane subsequently, acetic acid and formic acid to be removed as penetrant
Go, with re-using in method.
Green Extraction Technology grading plant is used to make biomass stand high-frequency impulse and shearing subsequently
Power, and do not make lignin degeneration and/or degraded, the U.S. Application No. 14/454 that described device was submitted on August 8th, 2014,
Described in 833.Within the most about 15 to about 30 seconds under the pulse of 912 to 1824, carry out classification biomass, to provide the first classification biological
Matter and the first liquid fraction.The first classification biomass are made to contact, so that pH is raised to about 9 with 0.3% w:w sodium hydroxide based on water
Above.The first classification biomass are made to stand compression stress subsequently, will have the second liquid level of most of remaining hemicellulose
The second classification biomass high with cellulose and content of lignin are divided to separate.
The second classification biomass are made to stand oxidation, to be separated with cellulose by lignin subsequently.Form oxidation mixture, and
It comprises 2000ml and uses 60g sodium hydroxide and 3% hydrogen peroxide of 300ml acetate buffer.By by 2g sodium carbonate stabilizer and
15mg powder manganese amino-acid chelate catalyst is mixed to form catalyst/stabilizer blend.By powder catalyst/stable
Agent composition is applied in the second classification biomass, and makes it contact with liquid oxidatively mixture subsequently, and aoxidizes 60 minutes.Make
Make the second oxidized classification biomass stand compression stress with the Double helix forcing press with stirring, have less than 7% to provide
The 3rd classification biomass that the content of cellulose of content of lignin is high and high the 3rd liquid fraction of water-soluble lignin content.With
Rear use 1500 ml hydrogen peroxide and other component of same amount of oxidation mixture and catalyst/stabilizer blend make
Three classification biomass reoxidation 60 minutes.Make the 3rd oxidized classification biomass stand compression stress subsequently, have to provide
The 4th classification biomass that the content of cellulose of the content of lignin less than 7% is high and high the 4th liquid fraction of content of lignin.
Repeat whole oxidizing process subsequently, use 1000ml hydrogen peroxide oxidation 120 minutes, and be then subjected to compression stress, to provide tool
There are the 5th classification biomass that the content of cellulose of the content of lignin less than 5% is high.
Analyze the contact of percentage ratio lignin, Kappa number and the fiber quality of wheat straw classification biomass.Result provides at table 1
In.
Table 1
。
Embodiment 4
Wild oat is used to repeat embodiment 3.Analyze lignin contact and the Kappa number of wild oat classification biomass.Result provides
In table 2.
Table 2
。
Embodiment 5
Repeat embodiment 2, except using 1000 ml hydrogen peroxide to make the 5th classification biomass of oxidation be again subjected to oxidation.With
After make this paper pulp and north bleached softwood wood sulfate pulp (" NBSK ") with the paper pulp/20%NBSK blend group of 80% present invention
Close, be added to 8% calcium carbonate.It is made into paper, to simulate inkjet type paper.
Embodiment 6
Repeat embodiment 3, except using 1000 ml hydrogen peroxide to make the 5th classification biomass of oxidation be again subjected to oxidation.With
After make this paper pulp and north bleached softwood wood sulfate pulp (" NBSK ") with the paper pulp/20%NBSK blend group of 80% present invention
Close, be added to 8% calcium carbonate.It is made into paper, to simulate inkjet type paper.
Table 3 provides the test of the paper that commercially available inkjet type paper prepared with respect to embodiment 5 and 6.
This display is compared with comparison paper, and the paper of the present invention has significantly higher intensity and toughness, owing to using this
The method of invention avoids and makes cellulose degeneration and/or degraded.
Although the present invention being had been disclosed for illustrative purposes be chosen for embodiment, but those skilled in the art will
Recognize and may carry out various amendment, add and replace, without departing from present invention disclosed the most in the dependent claims
Scope and spirit.
Claims (8)
1., for the method providing the cellulose from biomass isolation, described method includes:
A) described biomass are carried out pretreatment；
B) make described pretreated biomass stand high-frequency impulse and shearing force, and do not make the individual components of described biomass
Degeneration and/or degraded；
C) described biomass are made to stand compression stress, the first liquid fraction to be separated with the first classification biomass；
D) make described first classification biomass stand condition so that pH rises to more than 9, and make described biomass stand and step subsequently
Rapid b) identical high-frequency impulse and shearing force；
E) described first classification biomass are made to stand compression stress, so that the second liquid fraction is separated with the second classification biomass, its
Described in the second classification biomass substantially free from hemicellulose and sugar；
F) make to stand oxidation under described the second classification biomass substantially free from hemicellulose and sugar pH more than 7；With
G) described second classification biomass are made to stand compression stress, one or more of to separate from described second classification biomass
Water-soluble component, comprises the 3rd classification biomass of cellulose to provide, and described cellulose is substantially free from hemicellulose, sugared and wooden
Quality.
2. the method described in claim 1, farther includes after step e):
Make described second classification biomass be again subjected to condition so that pH rises to more than 9, and make described second classification biomass warp
Power by compression, to separate one or more of water-soluble component from described second biomass.
3. the method described in claim 1, wherein carries out described step at ambient temperature to about 60 DEG C.
4. the method described in claim 1, farther includes after step g):
H) make under described 3rd classification biomass pH more than 7, to stand oxidation；With
I) described 3rd classification biomass are made to stand compression stress, to separate one or more of water solublity group from described biomass
Point, to provide the 4th classification biomass comprising cellulose, described cellulose is substantially free from hemicellulose, sugar and lignin.
5. there is the cellulose less than 7% lignin, its not degeneration and/or fall due to extreme temperature, pressure or electrochemical conditions
Solve.
6. by prepared by the method described in claim 1, there is the cellulose less than 7% lignin, its not due to extreme temperature,
Pressure or electrochemical conditions and degeneration and/or degraded.
7. paper or paper products, are prepared by the cellulose described in claim 5.
8., for the method providing the cellulose from biomass isolation, stand condition with from described biomass including making biomass
Separate cellulose, to provide the fraction comprising cellulose and lignin, and do not make described cellulose degeneration or degraded, and oxygen subsequently
Change described fraction, to provide, there is the cellulose less than 7% lignin.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US14/454,972 US20150045543A1 (en) | 2013-08-12 | 2014-08-08 | Isolation method for water insoluble components of a biomass and products provided therefrom |
| US14/454972 | 2014-08-08 | ||
| PCT/US2015/015368 WO2016022172A1 (en) | 2013-08-12 | 2015-02-11 | Method for isolating cellulose from a biomass and products provided therefrom |
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| Publication Number | Publication Date |
|---|---|
| CN105980630A true CN105980630A (en) | 2016-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201580002207.5A Pending CN105980630A (en) | 2014-08-08 | 2015-02-11 | Method for isolating cellulose from a biomass and products provided therefrom |
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| EP (1) | EP3177768A1 (en) |
| CN (1) | CN105980630A (en) |
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| CN110983846A (en) * | 2019-12-19 | 2020-04-10 | 蚌埠产品质量监督检验研究院 | Preparation method of sisal cellulose whisker, non-woven fabric for filter and preparation method |
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| EP3177768A1 (en) | 2017-06-14 |
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