US2015247009A1PendingUtilityA1

Method for isolating lignin from a biomass and products provided therefrom

Assignee: MITCHELL MELVINPriority: Aug 12, 2013Filed: Feb 11, 2015Published: Sep 3, 2015
Est. expiryAug 12, 2033(~7 yrs left)· nominal 20-yr term from priority
C08B 15/08C08H 8/00D21C 3/224D21H 11/00C08G 63/912D21C 3/02C08B 37/0057C08H 6/00D21C 1/02C08G 63/06H01R 13/6594H01R 13/6273H01R 24/60H05K 5/0069H01R 13/6272
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Claims

Abstract

The process includes pretreating the biomass to provide a fluidized biomass. The fluidized biomass is then subjected to high frequency pulses and shear forces without denaturing/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 such as with hydrogen peroxide and base at a pH above 7. The second fractioned biomass is then subjected to compressive forces to provide water soluble lignin which may be precipitated by reducing the pH.

Claims

exact text as granted — not AI-modified
That which is claimed is: 
     
         1 . A process for isolating lignin from a biomass in water soluble form and a biomass substantially devoid of hemicellulose, sugar and the water insoluble components, the process comprising:
 a) pretreating the biomass;   b) subjecting the pretreated biomass to high frequency pulses and shear forces without denaturing/degrading the individual components of the biomass;   c) subjecting the biomass to compressive force to separate a first liquid fraction from a first fractionated biomass;   d) subjecting the first fractionated biomass to the same high frequency pulses and shear forces of step b);   e) subjecting the first fractionated biomass to compressive forces to separate a second liquid fraction from a second fractionated biomass wherein the second fractionated biomass is substantially devoid of hemicelluloses and sugars;   f) subjecting the second fractionated biomass substantially devoid of hemicelluloses and sugars to oxidation at a pH above 7; and   g) subjecting the second fractionated biomass to compressive force to separate lignin in water soluble form from the second fractionated biomass, wherein the lignin is substantially devoid of hemicellulose, sugar and the water insoluble components of the biomass.   
     
     
         2 . The process of  claim 1 , further comprising after step e) contacting the second fractionated biomass substantially devoid of hemicelluloses and sugars with a second basic solution and subjecting the second fractionated biomass to compressive force to separate at least one first water insoluble component of a biomass in water soluble form from the second fractionated biomass substantially devoid of hemicelluloses and sugars. 
     
     
         3 . The process of  claim 2 , wherein the first and second basic solutions comprise sodium hydroxide. 
     
     
         4 . The process of  claim 1  wherein the steps are conducted at ambient temperature to about 60° C. 
     
     
         5 . The process of  claim 1  wherein step f) of subjecting the second fractionated biomass substantially devoid of hemicelluloses and sugars to oxidation included contacting the second fractionated biomass substantially devoid of hemicelluloses and sugars with a hydrogen peroxide solution. 
     
     
         6 . The process of  claim 1 , wherein the water insoluble component of a biomass in water soluble form is purified by contacting with a membrane. 
     
     
         7 . A water insoluble component of a biomass in water soluble form provided by the method  claim 1 . 
     
     
         8 . A process for providing lignin of a biomass and a biomass substantially devoid of hemicellulose, sugar and the water insoluble components, the process comprising:
 a) pretreating the biomass;   b) subjecting the pretreated biomass to high frequency pulses and shear forces without denaturing the individual components of the biomass;   c) subjecting the biomass to compressive force to separate a first liquid fraction from a first fractionated biomass;   d) monitoring the amount of hemicellulose in the first fractionated biomass to determine if first fractionated biomass substantially devoid of hemicellulose and sugar,   e) subjecting the first fractionated biomass, if not devoid of hemicellulose and sugar to the same high frequency pulses and shear forces of step b);   f) subjecting the first fractionated biomass to compressive forces to separate a second liquid fraction from a second fractionated biomass wherein the second fractionated biomass is substantially devoid of hemicelluloses and sugars;   g) subjecting the second fractionated biomass substantially devoid of hemicellulose and sugars to oxidation at a pH above 7; and   h) subjecting the second fractionated biomass following oxidation to compressive forces to separate one or more water insoluble components of a third fractionated biomass and to provide a third liquid fraction comprising lignin in water soluble form substantially devoid of hemicellulose, sugar and the water insoluble components of the biomass.   
     
     
         9 . The process of  claim 8 , further comprising after step h):
 i) subjecting the third liquid fraction comprising lignin in water soluble form to a precipitation step comprising adjusting the pH of said liquid fraction to a pH of less than about 5.0 to provide precipitated lignin.   
     
     
         10 . The process of  claim 8 , further comprising after step h):
 i) subjecting the third fractionated biomass to oxidation at a pH above 7;   j) subjecting the third fractionated biomass following oxidation to compressive forces to separate one or more water insoluble components of a fourth fractionated biomass and to provide a fourth liquid fraction comprising lignin in water soluble form; and   k) combining the third and fourth liquid fractions to provide lignin in water soluble form substantially devoid of hemicellulose, sugar and the water insoluble components of the biomass.   
     
     
         11 . The process of  claim 10 , further comprising after step k):
 l) subjecting the combined fractions comprising lignin in water soluble form to a precipitation step comprising adjusting the pH of said liquid fraction to a pH of less than 4.0 to provide precipitated lignin.   
     
     
         12 . The process according to  claim 1 , wherein the organic solvent is selected from the group consisting of methanol, ethanol, propanol, butanol, and glycol. 
     
     
         13 . The process according to  claim 1 , wherein the solvent is any one selected from a group consisting of a short chain alcohol, glycerin and water, or a co-solvent mixture of any combination thereof. 
     
     
         14 . A lignin that is substantially the same as prior to isolation from a biomass wherein the lignin is high in molecular weight and has not been denatured or degraded during delignification of the biomass. 
     
     
         15 . The lignin of  claim 14  having a molecular weight mean greater than 10,000. 
     
     
         16 . A lignin that is substantially the same as prior to isolation from a biomass wherein the lignin is high in molecular weight and has not been denatured or degraded during delignification of the biomass prepared by the process of  claim 1 . 
     
     
         17 . A lignin that is substantially the same as it was prior to isolation from a biomass wherein the lignin is high in molecular weight and has not been denatured or degraded during delignification of the biomass prepared by the process of  claim 8 . 
     
     
         18 . A polymer or copolymer comprising the lignin of  claim 14 . 
     
     
         19 . The polymer or copolymer of  claim 18 , wherein polymer or copolymer comprises PLA. 
     
     
         20 . A carbon or graphite fiber, carbon fiber reinforced polymer or a carbon nanotube comprising the lignin of  claim 14 . 
     
     
         21 . A deconstruction product of the lignin of  claim 14 . 
     
     
         22 . The deconstruction product of  claim 21 , wherein the product is selected from the group consisting of phenols, cresols, catechols, resorcinols, quinolines, vanillin, guaiacols, cinnamic acid, p-coumaric acid, caffeic acid, ferulic acid, sinapic acid andp-hydroxycinnamic acid. 
     
     
         23 . A process for providing lignin isolated from a biomass comprising subjecting a biomass to conditions to separate cellulose and lignin from the biomass to provide a fraction comprising cellulose and lignin without denaturing or degrading the cellulose or lignin, oxidizing the fraction, and separating the cellulose from the lignin.

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