# US 2014/0155301 A1 · Processes and apparatus for producing nanocellulose, and compositions and products produced therefrom

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- Number: US 2014/0155301 A1
- Document ID: US20140155301A1
- Status: Published application
- Kind: A1
- Application number: 14/092,908
- Filed: 2013-11-27
- Published: 2014-06-05
- Earliest claimed: 2012-11-30
- Assignees: API Intellectual Property Holdings, LLC
- Applicants: API Intellectual Property Holdings, LLC
- Inventors: Kimberly NELSON; Theodora RETSINA; Vesa PYLKKANEN; Ryan O'CONNOR
- Web page: https://patentgrep.com/patent/US20140155301A1

## CPC

- C08B 15/08: Fractionation of cellulose, e.g. separation of cellulose crystallites
- C07G 1/00: Low-molecular-weight derivatives of lignin (high-molecular-weight derivatives of lignin {C08H6/00})
- C08B 15/00: Preparation of other cellulose derivatives or modified cellulose {, e.g. complexes}
- C08B 15/02: Oxycellulose; Hydrocellulose; {Cellulosehydrate, e.g. microcrystalline cellulose}
- C08B 37/0057: {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}
- C08H 8/00: Macromolecular compounds derived from lignocellulosic materials {(pretreatment thereof B27N)}
- C08L 1/02: Cellulose; Modified cellulose
- C12P 7/04: acyclic
- C12P 7/10: substrate containing cellulosic material
- C12P 7/14: Multiple stages of fermentation; Multiple types of microorganisms or re-use of microorganisms
- C12P 7/16: Butanols
- C12P 7/28: Acetone-containing products
- C12P 7/46: Dicarboxylic acids having four or less carbon atoms, e.g. fumaric acid, maleic acid
- C12P 7/56: Lactic acid
- C12P 19/02: Monosaccharides (2-ketogulonic acid C12P7/60)
- C12P 19/14: produced by the action of a carbohydrase {(EC 3.2.x)}, e.g. by alpha-amylase {, e.g. by cellulase, hemicellulase}
- C13K 1/02: obtained by saccharification of cellulosic materials (manufacture of fodder A23K10/32)
- D21C 3/04: with acids, acid salts or acid anhydrides {(D21C3/003 and D21C3/222 take precedence)}
- D21C 3/06: sulfur dioxide; sulfurous acid; bisulfites {sulfites}
- D21C 3/20: with organic solvents {or in solvent environment}
- D21C 5/00: Other processes for obtaining cellulose, e.g. cooking cotton linters (obtaining fibres for spinning D01C); {Processes characterised by the choice of cellulose-containing starting materials}
- D21C 5/005: {Treatment of cellulose-containing material with microorganisms or enzymes}
- D21C 9/002: {by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives}
- D21C 9/007: {by mechanical or physical means}
- D21C 9/10: Bleaching {; Apparatus therefor}
- D21C 11/0007: {Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for (volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042)}
- D21H 11/18: Highly hydrated, swollen or fibrillatable fibres
- C12P 2201/00: Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
- C12P 2203/00: Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
- Y02E 50/10: Biofuels, e.g. bio-diesel
- Y02P 40/40: Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)
- C07G: COMPOUNDS OF UNKNOWN CONSTITUTION (sulfonated fats, oils or waxes of undetermined constitution C07C309/62)
- C08H: DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS (polysaccharides C08B; natural rubber C08C; natural resins or their derivatives C09F; bituminous materials C10)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)}
- C13K: SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES (chemically synthesised sugars or sugar derivatives C07H; polysaccharides, e.g. starch, derivatives thereof C08B; malt C12C; fermentation or enzyme-using processes for preparing compounds containing saccharide radicals C12P19/00; production of sucrose C13B)
- D21C: PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- 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
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Processes disclosed are capable of converting biomass into high-crystallinity nanocellulose with surprisingly low mechanical energy input. In some variations, the process includes fractionating biomass with an acid (such as sulfur dioxide), a solvent (such as ethanol), and water, to generate cellulose-rich solids and a liquid containing hemicellulose and lignin; and mechanically treating the cellulose-rich solids to form nanofibrils and/or nanocrystals. The total mechanical energy may be less than 500 kilowatt-hours per ton. The crystallinity of the nanocellulose material may be 80% or higher, translating into good reinforcing properties for composites. The nanocellulose material may include nanofibrillated cellulose, nanocrystalline cellulose, or both. In some embodiments, the nanocellulose material is hydrophobic via deposition of some lignin onto the cellulose surface. Optionally, sugars derived from amorphous cellulose and hemicellulose may be separately fermented, such as to monomers for various polymers. These polymers may be combined with the nanocellulose to form completely renewable composites.

## Claims

### Claim 1

A nanocellulose composition comprising nanofibrillated cellulose with a cellulose crystallinity of about 70% or greater.

### Claim 2

A nanocellulose composition comprising nanofibrillated cellulose and nanocrystalline cellulose, wherein said nanocellulose composition is characterized by an overall cellulose crystallinity of about 70% or greater.

### Claim 3

A nanocellulose composition comprising nanocrystalline cellulose with a cellulose crystallinity of about 80% or greater, wherein said nanocellulose composition comprises lignin and sulfur.

### Claim 4 (depends on 1, 2)

The nanocellulose composition of either of claim 1 or 2, wherein said cellulose crystallinity is about 75% or greater.

### Claim 5 (depends on 4)

The nanocellulose composition of claim 4, wherein said cellulose crystallinity is about 80% or greater.

### Claim 6 (depends on 3, 4)

The nanocellulose composition of either of claim 3 or 4, wherein said cellulose crystallinity is about 85% or greater.

### Claim 7 (depends on 1, 2)

The nanocellulose composition of either of claim 1 or 2, wherein said nanocellulose composition comprises lignin.

### Claim 8 (depends on 1, 2)

The nanocellulose composition of either of claim 1 or 2, wherein said nanocellulose composition comprises sulfur.

### Claim 9 (depends on 1, 2, 3)

The nanocellulose composition of any of claims 1-3, wherein said nanocellulose composition is not derived from tunicates.

### Claim 10 (depends on 1, 2, 3)

The nanocellulose composition of any of claims 1-3, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 100 to about 1000.

### Claim 11 (depends on 10)

The nanocellulose composition of claim 10, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 300 to about 700.

### Claim 12 (depends on 10)

The nanocellulose composition of claim 10, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 150 to about 250.

### Claim 13 (depends on 1, 2, 3)

The nanocellulose composition of any of claims 1-3, wherein said nanocellulose composition is characterized by a cellulose degree of polymerization distribution having a single peak.

### Claim 14 (depends on 1, 2, 3)

The nanocellulose composition of any of claims 1-3, wherein said nanocellulose composition is free of enzymes.

### Claim 15

A hydrophobic nanocellulose composition with a cellulose crystallinity of about 70% or greater, wherein said nanocellulose composition contains nanocellulose particles having a surface concentration of lignin that is greater than a bulk concentration of lignin.

### Claim 16 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said cellulose crystallinity is about 75% or greater.

### Claim 17 (depends on 16)

The hydrophobic nanocellulose composition of claim 16, wherein said cellulose crystallinity is about 80% or greater.

### Claim 18 (depends on 17)

The hydrophobic nanocellulose composition of claim 17, wherein said cellulose crystallinity is about 85% or greater.

### Claim 19 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said nanocellulose composition further comprises sulfur.

### Claim 20 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said nanocellulose composition is not derived from tunicates.

### Claim 21 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 100 to about 1500.

### Claim 22 (depends on 21)

The hydrophobic nanocellulose composition of claim 21, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 300 to about 700.

### Claim 23 (depends on 21)

The hydrophobic nanocellulose composition of claim 21, wherein said nanocellulose composition is characterized by an average cellulose degree of polymerization from about 150 to about 250.

### Claim 24 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said nanocellulose composition is characterized by a cellulose degree of polymerization distribution having a single peak.

### Claim 25 (depends on 15)

The hydrophobic nanocellulose composition of claim 15, wherein said nanocellulose composition is free of enzymes.

### Claim 26 (depends on 1, 2, 3)

A nanocellulose-containing product comprising the nanocellulose composition of any one of claim 1, 2, 3, or 15.

### Claim 27 (depends on 26)

The nanocellulose-containing product of claim 26, wherein said nanocellulose-containing product is selected from the group consisting of a structural object, a foam, an aerogel, a polymer composite, a carbon composite, a film, a coating, a coating precursor, a current or voltage carrier, a filter, a membrane, a catalyst, a catalyst substrate, a coating additive, a paint additive, an adhesive additive, a cement additive, a paper coating, a thickening agent, a rheological modifier, an additive for a drilling fluid, and combinations or derivatives thereof.