WO2001032715A1 - Procede de production de produits organiques a partir de sources de biomasses diverses contenant de la lignocellulose - Google Patents

Procede de production de produits organiques a partir de sources de biomasses diverses contenant de la lignocellulose Download PDF

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Publication number
WO2001032715A1
WO2001032715A1 PCT/US2000/030438 US0030438W WO0132715A1 WO 2001032715 A1 WO2001032715 A1 WO 2001032715A1 US 0030438 W US0030438 W US 0030438W WO 0132715 A1 WO0132715 A1 WO 0132715A1
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hydrolysis
stage
fermentation
dilute acid
reactor
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PCT/US2000/030438
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English (en)
Inventor
Charles K. Lombard
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Waste Energy Integrated Sytems, Llc
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Priority to AU15842/01A priority Critical patent/AU1584201A/en
Publication of WO2001032715A1 publication Critical patent/WO2001032715A1/fr

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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
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
    • C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration
    • C13B20/165—Purification of sugar juices by physical means, e.g. osmosis or filtration using membranes, e.g. osmosis, ultrafiltration
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic 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
    • D21C1/04—Pretreatment of the finely-divided materials before digesting with acid reacting compounds
    • 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
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/582—Recycling of unreacted starting or intermediate materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the present invention relates to the production of useful organic products from diverse biomass.
  • the invention relates to the large-scale production of organic products such as sugars, ethanol, lignan and derivative biodegradable thermoplastics from agricultural, forestry and municipal wastes, in an energy efficient and environmentally sensitive manner.
  • MSW Mixed municipal solid waste
  • composting particularly of source separated "greenwaste” that includes yard waste, vegetable material and mixed waste paper.
  • Composting involves natural aerobic fermentation under the action of bacteria, yeast and fungal organisms and their enzymes that in commercial practice degrade principally the carbohydrate and hemicellulose polysaccharide components of biomass.
  • US Patent No. 5,326,477 to Fuqua et al. describes a process directed toward volume reduction and sewage disposal of certain high cellulose content solid waste, such as disposable diapers and pads, by liquefaction through enzymatic breakdown in a cellulase solution.
  • the process conditions given are such as to support rapid, partial fragmentation of the cellulosic polymer chains sufficient to render the material suitable for liquid transportable discharge through a pipe. Provision is made to capture a plastic shell (film) for prospective recycling.
  • US Patent No. 5,705,216 to Tyson discloses methods of alkaline pulping using a mechanical extruder to crush and feed NaOH-soaked biomass wastes, such as wood and agricultural residues, into a pressure chamber where, under the action of saturated steam in the 200°C regime, the material is digested for several minutes. Tyson's process is terminated by sudden pressure release (steam explosion) on the digested material as it exits the extruder. The process, with variants, is directed to the partial solubilization of lignin and hemicellulose and the disruption of the lignocellulosic matrix of biomass with the principal purpose of creating a reactive, absorbent, fibrous material.
  • This product aims to serve a variety of purposes from ruminant animal feed to composite alternative structural materials (with or without the addition of recycled thermoplastics).
  • Another aim of the invention is to extract from the treated fiber a solubilized portion of the polymeric constituents lignin and hemicellulose, together comprising an extractable weight reduction of about 32% of the feedstock material.
  • hemicellulose and lignin together comprise about 50% of biomass feedstock materials, h Tyson's process, the extracted portion of the hemicellulose is optionally available to subsequent enzymatic hydrolysis to sugars with prospective fermentation to ethanol and organic acids.
  • US Patent No. 4,728,367 to Huber describes an extruder device and a process for either strong or dilute acid pretreatment directed toward providing partial solubilization and hydrolysis of hemicellulose from lignocellulosic materials. Under comparatively elevated temperatures and pressures and very short acid contact times of several seconds, Huber indicates glucose production of a modest 13-20% of feedstock.
  • the Brink patent gives a two-stage dilute acid hydrolysis process preferably with nitric acid and carried out under saturated steam in a pressure reactor.
  • the first stage hydrolysis is performed under comparatively mild conditions of pH (about 2), temperature (about 185° C) and pressure (about 10 atmospheres).
  • the aim of the first stage is to solubilize, hydro lyze and extract most of the hemicellulose from the lignocellulosic matrix while not substantially degrading the cellulose and liberated monomeric sugars. This aim is achieved in several minutes digestion time with the result of solubilizing and enabling the extraction of about 30% of the biomass feedstock material, leaving lignin and much of the cellulose intact.
  • the Brink process After acting to separate the solubilized five- and six-carbon sugars of the hemicellulose, the Brink process then addresses the more difficult issue of hydrolysis and solubilization of the cellulose polysaccharide under more extreme conditions of lower pH, temperature over 200° C and pressure 20 atmospheres for over 10 minutes. Under carefully tailored conditions for a given homogeneous feedstock, sugar production and degradation can be optimized to yield a total about 60%> of potential sugars in the two-stage dilute acid process.
  • Patent No. 5,628,830 to Brink ('830 patent).
  • the patent describes an alternative process directed toward increasing sugar and ethanol yield through a second hydrolysis of the lignocellulosic solids from the first stage by enzymatic digestion.
  • Relative to Brink's '903 patent his enzymatic process replaces the second stage dilute acid hydrolysis of cellulose under more severe conditions than the first stage hydrolysis of hemicellulose.
  • the '830 patent reveals that, with the combined mechanical refinement and steam explosion disintegration, a preponderance of the solid particles is smaller than about 100 mesh for typical woody substrates.
  • the '830 patent description reveals that, at cellulase enzyme loading of about 13.5 FPU/gm on mixed New York hardwood substrate, at low, and with about 5% solids loading in aqueous carrier, the process-implemented batch simultaneous saccharification and fermentation (SSF) with S. cereviseae yeast is capable to yield 89.2%o cellulose-to-ethanol conversion in 4 days.
  • SSF process-implemented batch simultaneous saccharification and fermentation
  • the combination of low solids loading and SSF fermentation act together to limit buildup of sugar concentrations in the reactor and contain so-called end product inhibition of enzymatic hydrolysis. Accordingly, Brink's results indicate a significant speedup in batch enzymatic hydrolysis of dilute acid pretreated lignocellulose solids substrate vis-a-vis the comparative literature, heretofore.
  • US Patent 5,036,005 to Tedder describes an invention directed toward efficient, continuous fermentation of sugars with continuous solvent extraction of both ethanol and volatile organic coproducts from a biocatalyst-containing fermentation broth.
  • the invention poses the opportunity to economically recover volatile organic coproducts and ethanol with low expenditure of energy and capital cost, while also avoiding additional investment in drying to fuel grade ethanol.
  • the tightly integrated system requires the use of a solvent that conventionally has a higher boiling point than the products to be extracted and also is nontoxic to the fermentation organisms the solvent intimately contacts. The latter constraint obviates the use of otherwise attractive higher alcohols as solvents.
  • the present invention achieves further advances in biomass processing by providing processes and systems for the increased production of useful organic products from diverse lignocellulose-containing biomass.
  • the present invention integrates dilute acid hydrolysis and alkaline delignification techniques in processes that enhance the quantity of products, i.e., material utilization efficiency and yield, of lignocellulostic biomass processing and enable the economic production lignin-based biodegradable plastics and other useful organic products.
  • the invention integrates technologies in chemical processing to achieve exceptional product yields, value added and productivity in the production of sugars, ethanol, lignin, other (photosynthetically) plant-derived organic chemicals, and process-derived biocatalyst proteins from a diverse spectrum of commonly occurring biomass sources. These prominently include wastes (residues) of agricultural, forest/mill and municipal origin. Synergistically sharing process costs while supporting (maximizing) added value in multiple products, the invention poses the prospect to newly render highly cost-effective the large-scale remanufacture (reuse) of the organic products of human activities.
  • Processes in accordance with the present invention may also prominently feature environmentally benign attributes of energy efficiency, material (e.g., water) conservation and avoids chemical nuisance/ toxicity, which, together with the theme of renewable materials products, contribute to the objectives of sustainable ecology.
  • material e.g., water
  • the present invention provides a method of processing a lignocellulose-containing biomass material.
  • the method involves treating the biomass material by dilute acid hydrolysis and treating an unreacted lignocellulostic component of the acid hydrolyzed biomass material by alkaline delignification.
  • these processing techniques will be combined with others to provide for efficient, high-yield processing of lignocellulostic biomass.
  • Other aspects of the invention also provide systems configured for processing a lignocellulose-containing biomass material in accordance with the method of the present invention.
  • Fig. 1 is a flow chart depicts aspects of a process flow in accordance with a preferred embodiment of the present invention.
  • Figs. 2 and 3 are schematic illustrations of process flows for the production of organic products from diverse lignocellulostic biomass sources in accordance with preferred embodiments of the present invention.
  • the present invention achieves advances in MSW processing by providing processes and systems for the production of useful organic products from diverse lignocellulose-containing biomass having increased yield and efficiency.
  • the present invention integrates dilute acid hydrolysis and alkaline delignification techniques in processes that enhance the material utilization efficiency and yield of lignocellulostic biomass processing.
  • the invention integrates technologies in chemical processing to achieve exceptional product yields, value added and productivity in the production of sugars, ethanol, lignin and derivative biodegradable thermoplastics, other (photosynthetically) plant-derived organic chemicals, and process-derived biocatalyst proteins from a diverse spectrum of commonly occurring biomass sources. These prominently include wastes (residues) of agricultural, forest/mill and municipal origin. Synergistically sharing process costs while supporting (maximizing) added value in multiple products, the invention poses the prospect to newly render highly cost-effective the large-scale remanufacture (reuse) of the organic products of human activities.
  • Processes in accordance with the present invention may also prominently feature environmentally benign attributes of energy efficiency, material (e.g., water) conservation and avoids chemical nuisance/ toxicity, which, together with the theme of renewable materials products, contribute to the objectives of sustainable ecology.
  • material e.g., water
  • Fig. 1 shows a flow chart depicting key stages in a biomass processing method 100 in accordance with the present invention.
  • a biomass feed material is provided to a biomass processing system (102).
  • the biomass is treated by dilute acid hydrolysis (104), for example, as further described below.
  • dilute acid hydrolysis 104
  • an unreacted lignocellulostic component of the acid hydrolyzed biomass material is treated by alkaline delignification (106).
  • alkaline delignification 106
  • these processing techniques are integrated with further processing techniques (108) such as filtration, internal process recycling, distillation, enzymatic hydrolysis, and bacterial and yeast fermentation in a comprehensive, continuous, high-yield process enabling the production of biodegradable thermoplastic and other useful organic products.
  • further processing techniques such as filtration, internal process recycling, distillation, enzymatic hydrolysis, and bacterial and yeast fermentation in a comprehensive, continuous, high-yield process enabling the production of biodegradable thermoplastic and other useful organic products.
  • the starting biomass feed material may be any organic matter, and is generally composed plant material, vegetation, agricultural, industrial or household waste. It may include, without limitation, include one or more of the following: wood, paper, straw, leaves, prunings, vegetable pulp, corn, corn stover, sugarcane, sugar beets, sorghum, cassava, potato waste, bagasse, sawdust and forest mill waste.
  • One common source of biomass feed material for processes in the nature of the present invention is derived from pre- or post-classified mixed municipal solid waste (MSW).
  • Lignocellulose is a combination of lignin, hemicellulose and cellulose polymers that strengthens woody plant cells.
  • the present invention is particularly well-suited to the processing of lignocellulose- containing biomass (also referred to herein as a lignocellulostic biomass).
  • Preferred embodiments of the present invention incorporate a continuous, interwoven chain of several continuous stages. These may be generically recognized from the biomass ethanol, chemical pulping and separation process literature as including: (1) dilute acid hydrolysis; (2) alkaline delignification; (3) enzymatic hydrolysis; (4) fermentation; and (5) product separation. As noted above, alternative embodiments of the invention may order and, in some cases, combine these stages and variations thereof to implement the invention. Two such embodiments are outlined and then described in detail below.
  • the present invention is implemented as a five stage process, as follows: (1) dilute acid hydrolysis (hemicellulose); (2) dilute acid hydrolysis (cellulose); (3) alkaline delignification; (4) bacterial fermentation; and (5) yeast fermentation combined with enzymatic hydrolysis.
  • this process also involves intertwined product separation and recovery and the recycling of useful process facilitators, such as water and enzymes. This embodiment is further described below with reference to Fig. 2.
  • a lignocellulose-containing biomass feedstock is prepared for processing using techniques well known to those of skill in the art.
  • the feedstock is ground, screened, and prewashed to remove parasitic dirt.
  • the dirt is settled and may be used for soil amendment.
  • the prewash water is recyled for subsequent use in the biomass processing.
  • the pre-processed biomass is then dewatered.
  • the dewatered biomass feedstock is subjected to an acid presoak under warm water conditions.
  • the use of nitric acid in the presoak and subsequent hydrolysis for example, reduces employee hazard and enables employing low-cost, corrosion- resistant stainless steel reactors.
  • the acid presoaked biomass is spun dry, and then further dried by solar/waste heat to about 50% solids.
  • Stage 1 Dilute Acid Hydrolysis (Hemicellulose)
  • the first stage of this process in accordance with the present invention involves dilute acid hydrolysis of cellulosic polymer chains in the pre-treated lignocellulosic biomass feedstock, using strong acids, such as nitric or sulfuric. The result is to hydrolyze, solubilize and substantially convert to monomeric sugars most of the polysaccharide constituents of hemicellulose and a small portion, most easily hydrolyzed fraction of cellulose contained in the lignocellulosic feedstock material.
  • Stage 1 of this embodiment involves dilute acid hydrolysis of the pre-treated biomass feedstock.
  • Exemplary conditions for this hydrolysis are about 0.4% HNO 3 , at about 195°C for about 5 minutes in a saturated steam environment within a pressure reactor such as is commonly employed in the pulping industry.
  • Stage 1 is preferably terminated by rapid pressure release (steam explosion) and will solubilize and liberate about one-third of the material of the feedstock. The liquid hydrolysate and solids are then washed and pressed.
  • a first product separation and recovery is conducted.
  • the Stage 1 liquid hydrolysate is washed and pressed repeatedly from the residual solids to recover about 95% of the liberated sugars, polysaccharide fragments and coproduct volatile organic compounds — such as acetic acid, furfural and hydroxymethylfurfural.
  • the resulting press liquid comprising nominally six times the biomass feed contains solubilized product in about 5%> concentration.
  • the liquid is conveyed to a reservoir from which it is passed through nanofiltration (NF) membranes with a standard molecular weight cutoff designed to concentrate and contain the sugars.
  • NF nanofiltration
  • the concentrated retentate from the NF separation contains the free sugars at nominally 20% concentration and polysaccharide fragments, which are conveyed to the Stage 4 bacterial fermentation process, to be described.
  • the NF permeate contains volatile organics, along with dilute acid catalyst.
  • the economics of the process may be enhanced by recycling the permeate back through the Stage 1 wash cycles in successive iterations of the process, conserving acid and accumulating and concentrating VOC coproducts prior to their recovery.
  • Stage 2 Dilute Acid Hydrolysis (Cellulose)
  • the lignin cellulose solids from the press of stage 1 are passed to Stage 2, a second dilute acid hydrolysis stage.
  • acid e.g., nitric (HNO ) (preferred), sulfuric or hydrocloric
  • Stage 2 is preferably terminated by rapid pressure release (steam explosion) and will solubilize and liberate about half of the material from the Stage 1 press. The hydrolysate and solids are then washed and pressed to about 50% solids.
  • Stage 2 dilute acid hydrolysis
  • the Stage 2 liquid hydrolysate is washed and pressed repeatedly from the residual solids to recover about 95% of the liberated sugars, oligosaccharide fragments, acid and additional coproduct volatile organic compounds — such as hydroxymethylfurfural.
  • the resulting press liquid is conveyed to a reservoir from which it is passed through nanofiltration (NF) membranes.
  • NF nanofiltration
  • the concentrated retentate from the NF separation contains the free sugars at nominally 20% concentration and polysaccharide and oligosaccharide fragments, which together are conveyed to the Stage 4 bacterial fermentation process, to be described.
  • the aqueous permeate of nanofiltration is effectively reconcentrated by vacuum distillation for recycling the acid catalyst to the hydrolysis process stages.
  • the reconcentrated catalyst will also be recognized to contain the solubilized fraction of volatile organic chemicals that are liberated by the hydrolysis process in approximately 5% concentration weight/weight at each step of the biomass processing.
  • VOCs may be extracted by fractional distillation, as noted above.
  • a further advantage of the two-stage dilute hydrolysis of this embodiment of the present invention is the economic efficiency obtained in temporal utilization of tankage. As the result of the two-stage dilute acid hydrolysis, the bulk of the cellulose in the biomass feedstock is effectively decomposed in order minutes rather than days, as has previously been the standard for enzymatic hydrolysis.
  • Stage 3 of the process employs chemical delignification of the lignocellulosic solids from the press of Stage 2. Chemistries of the pulp and paper industry that have not previously been integrated with acid dehydrolysis and used in connection with the processing of lignocellulostic biomass are adopted. The preferred embodiment for environmental benefits adopts sulfur-free alkaline delignification from so-called "alkaline pulping" chemistry. Stage 2 solids may be combined with about 4% strong base (such as alkali or other lignin-dissolving base) at about 210°C for about 4 minutes. The alkaline process may be effectively catalyzed by the use of accelerators such as anthraquinone and tetrahydroanthraquinone.
  • accelerators such as anthraquinone and tetrahydroanthraquinone.
  • the time constant for delignification decreases (e.g., in kraft pulping) by about a factor of two for each 8° C increase in temperature.
  • Such rapid temporal performance in delignification as provided here is jointly facilitated by choosing to operate toward the higher end of the temperature range, here also employed in dilute acid hydrolysis, with similarly rapid solubilization and extraction of the hemicellulose.
  • Stage 3 may electively be terminated by either steam explosion or more energy, conserving heat recovery decompression. The product of this stage is then washed and pressed to separate the soluble lignin from the remaining lignin/cellulose solids.
  • the introduced alkaline delignification stage importantly distinguishes a process in accordance with the present invention from the common practice of biomass ethanol technology involving only dilute acid pretreatment and enzymatic hydrolysis.
  • the presence of naturally occurring amounts of lignin with the cellulose in the enzyme recycle reactor results in major, noneconomic declines in enzyme productivity (from cycle to cycle of enzyme reuse against fresh substrate) (Lombard, Charles K., Project Manager, Waste Energy Integrated Systems. Techno-Economics of the WEIS Biomass Ethanol Process [Final Report for Project: Enzymatic Utilization of Cellulose in a Continuous Bimembrane Reactor]. National Renewable Energy Laboratory Subcontract No.
  • Lignin-based thermoplastics have adjustable mechanical properties over the range identified with polyethylene, polypropylene and polystyrene are, moreover, biodegradeable.
  • the plastics may be foamed, filmed, cast or extrusion- or injection- molded to satisfy a great variety of applications.
  • energy-intensive synthesis reactions and associated sources of chemical toxicity are avoided.
  • the production of the new plastic only requires a catalytic chemical reaction, e.g., methylation, at normal conditions of temperature and pressure.
  • a catalytic chemical reaction e.g., methylation
  • Stage 3 washed solids residue is fed back to Stage 2 for subsequent further dilute acid hydrolysis and Stage 3 alkaline delignification to thereby achieve near 100%> substrate conversion.
  • the concentrated hydrolysate sugars and oligosaccharides of Stages I and II are combined and the glucose and five-carbon sugars are fermented with Zymomonas mobilis bacterium in a Stage 4 continuous-flow cascade recycle reactor, blocking and recycling the bacterial catalyst at the outflow while the residual six-carbon sugars and oligosaccharides are passed through a microfilter to a second (yeast) fermenter, discussed below.
  • the ethanol and carbon dioxide products are separated and the remaining six-carbon sugars and oligosaccharides are concentrated by vacuum evaporative distillation from the Stage 4 fermentation reactor.
  • Stages 4 and 5 of the process bacterial fermentation of sugars, also takes place in a continuous recycle reactor comprised of vessels containing separately or jointly provision of biocatalytic agents for fermenting both the five- and six-carbon sugars liberated in Stages 1, 2 and 3 of the process.
  • the practice of Stages 4 and 5 is distinct from prior art in biomass ethanol technology in achieving very high yield with large gains in productivity in both time and tankage realized by: 1) implementing a continuous-flow reactor with feedstock replenishment and product extraction, while 2) employing microfiltration to retain biocatalyst in the reactor to speed the process and 3) optionally making provision for product extracting dilution water to control end-product inhibition in the fermentation process.
  • a nanofiltration membrane can be used to retain catalyst and concentrated sugars in the reactor, while passing residual aqueous carrier.
  • the use of the robust bacterium Zymomonas mobilis, genetically engineered to ferment five-carbon sugars as well as glucose, and the yeast Saccharomyces cervisiae together support rapid fermentation of all the six- carbon sugars liberated in the two cellulosic hydrolysis stages. Concentrating the substrate sugars to order 20%o in aqueous solution and retaining order 10%> biocatalyst loading against the substrate with vacuum evaporative extraction of ethanol and CO will realize mean fermentation volume utilization in about one day.
  • VOC coproducts are separated by fractional distillation from the accumulated concentrated VOCs of the Stages 1 and 2 hydrolysate (wash) filter permeate.
  • the residual acid may be neutralized with ammonia or other suitable base to produce, along with other residual mineral salts, a valuable nitrogen-rich fertilizer coproduct.
  • the use of an NF membrane in the Stage 5 reactor to retain concentrated sugars while accumulating the organic chemical products of hydrolysis represents the beginning of the last instance of intertwined product separation in the process.
  • a major objective of the invention is to build broad flexibility into lignocellulostic biomass processes with regard to value adding product diversity, while maintaining energy efficiency and clean, functional consistency in the face of the fact that many chemical products and coproducts of interest, such as the volatile organic components of the hydrolysate, will have boiling points greater than that of water. Indeed, these coproducts typically pose potential product yield of 17% and product revenues exceeding 20% against the major product, e.g., ethanol, from sugar fermentation, but would imply several times more energy to first boil off all the water for their recovery by traditional distillation.
  • major product e.g., ethanol
  • the solvent is chosen to be buoyant and not miscible in water.
  • the solvent is also of higher boiling point than both water and the volatile organic chemicals to be recovered.
  • the solvent employed in separation process is further chosen to have a partition coefficient close to unity for both ethanol and the volatile organic liquids.
  • the product separation and extraction of the process is then concluded with product separation and recovery through fractional distillation from the higher boiling solvent.
  • the solvent so depleted of product is then conservatively recycled back through the solvent extraction process to recover more volatile organic product.
  • the fact that the solvent is chosen both to be buoyant and insoluble in water allows the product-laden solvent to be readily separated from the water on the one hand and, on the other, the product extraction dilution water to be recycled substantially free of solvent back through the fermentation recycle reactor.
  • the recycling of dilution water ultimately recovers loss of product in incomplete single transfer from water to solvent.
  • the present invention is implemented as a five stage process, as follows: (1) dilute acid hydrolysis (hemicellulose); (2) alkaline delignification; (3) enzymatic hydrolysis; (4) fermentation ((a) bacterial fermentation and (b) yeast fermentation); and (5) vacuum evaporative extraction or solvent extraction.
  • this process also involves product separation and recovery and the recycling of useful process facilitators, such as water and enzymes. This embodiment is further described below with reference to Fig. 3.
  • a lignocellulose-containing biomass feedstock is prepared and pretreated for processing as described above with reference to Fig. 2.
  • this embodiment has as it's first stage a dilute acid hydrolysis of cellulosic polymer chains, using strong acids, such as nitric or sulfuric conducted according to similar conditions and parameters described above for Embodiment 1 (e.g., 0.4% HNO 3 , at about 210°C for about 4 minutes).
  • strong acids such as nitric or sulfuric conducted according to similar conditions and parameters described above for Embodiment 1 (e.g., 0.4% HNO 3 , at about 210°C for about 4 minutes).
  • the result is to hydrolyze, solubilize and substantially convert to monomeric sugars most of the polysaccharide constituents of hemicellulose and a small portion, most easily hydrolyzed fraction of cellulose contained in the lignocellulosic feedstock material.
  • Stage 1 liquid hydrolysate is washed and pressed repeatedly from the residual solids to recover about 95% of the liberated sugars, polysaccharide fragments and coproduct volatile organic compounds — such as acetic acid, furfural and hydroxymethylfurfural.
  • the resulting press liquid comprising nominally six times the biomass feed contains solubilized product in about 5%o concentration.
  • the liquid is conveyed to a reservoir from which it is sequentially passed through microfiltration membranes as in the first embodiment.
  • the retentate from the NF separation contains sugars and polysaccharide fragments which are conveyed to the Stage 4 fermentation process as in Embodiment 1.
  • the NF permeate which contains the residual acid and volatile organics, is then recycled in the wash to concentrate and accumulate the VOCs through successive iterations of the process prior to accumulated product recovey by fractional distillation.
  • the sugars are concentrated to order 20% for efficient fermentation in Stage 4, to be described.
  • Stage 2 of this embodiment employs chemical delignification of the lignocellulosic solids, according to the methods described above for Stage 3 of Embodiment 1.
  • the introduced alkaline delignification stage importantly distinguishes a process in accordance with the present invention from the common practice of biomass ethanol technology involving only dilute acid pretreatment and enzymatic hydrolysis.
  • a major issue and objective of preferred implementations of the present invention is to provide for continuous material replenishment along with both needed mixing of the reactor contents while retaining an ordered separate sense of temporal aging of materials in the reactor.
  • the latter supports the ability to conveniently remove such aged, less reactive and relatively residual-lignin-enriched material in a discriminating manner.
  • a second major issue is how to concurrently provide wide latitude for reactor volume expansion (design) in a continuous-flow configuration while providing conveniently effective local control of dilution water limiting product buildup and end product inhibition in the reactor.
  • the effective solution practiced in accordance with this embodiment of the present invention is to decouple geometrically the functions (and directions) of material flow control and control of dilution water and product extraction in the enzyme recycle hydrolysis reactor.
  • the solution is practiced by adopting a new substantially horizontal channel configuration for the enzymatic hydrolysis reactor.
  • the substrate material flow independently takes place in the horizontal direction along the sense of length of the channel.
  • Separate provision for dilution water and product extraction can be independently facilitated crossflow (in the material sense) in either or both the width and depth directions, whose dimensions are freely adjustable relative to channel length.
  • Mixing to promote efficient redistribution of biocatalyst on substrate and incorporation of product sugars into dilution water for extraction can naturally be facilitated to take place locally on a scale of the shorter of channel width or depth.
  • the channel geometry provides for effective modular decomposition of scale of design by, for example, replicating parallel channels in the width and/or depth dimensions.
  • microfiltration devices positioned at or near the lateral (vertical or horizontal) boundaries.
  • the microfiltration blocks (retain or return to the channel) the cellulosic particulate substrate while the permeate contains freely floating enzymes and product sugars dissolved in the dilution water for subsequent UF and NF filtration with reduced fouling.
  • the second instance of the intertwined product separation process of Stage 5 is invoked.
  • the dilution water extracted from the enzymatic hydrolysis reactor is first nanofiltered through a membrane such as previously employed for the diluted hydrolysate of Stage 1.
  • the freely floating enzyme is collected in the retentate of the UF membrane and returned to the enzyme recycle reactor for reuse.
  • the permeate of UF membrane contains the product sugars of the enzyme recycle hydrolysis reactor. These are next concentrated in the retentate of an NF membrane preparatory to Stage 4 fermentation as otherwise employed for the diluted hydrolysate sugars of Stage 1 of the present process.
  • the enzyme biocatalyst employed in the hydrolysis reactor will in generality be composed of a combination of cellulases, hemicellulases, amylases and ligninases and these may be either introduced or produced in situ.
  • the continuous-flow hydrolysis reactor is operated at comparatively high substrate solids loading of from nominally 5% to 35%.
  • Moderate enzyme loading is in the range of about 1 to 35 FPU/gm substrate.
  • Volume dilution rate is about 0.1 to 1 per hour.
  • substrate loading is about 20%
  • enzyme loading is about 10 FPU/gm
  • dilution rate for product extraction is about 1 per hour.
  • the highly productive mean time for volume conversion of cellulose to sugar in the reactor is about one day.
  • Stage 4 of the present process fermentation of sugars, also takes place in a continuous recycle reactor comprised of vessels containing separately or jointly provision in biocatalytic agents for fermenting both the five- and six-carbon sugars liberated in Stages 1 and 3 of the present process.
  • the practice of Stage 4 is distinct from previous approaches used in biomass ethanol technology in achieving very high yield with large gains in productivity in both time and tankage realized by: 1) implementing a continuous-flow reactor with feedstock replenishment and product extraction, while 2) employing microfiltration and NF to retain biocatalyst and concentrated feedstock sugars in the reactor to speed the process, and 3) making provision for product extracting dilution water to control end product inhibition in the fermentation process.
  • the yeast reactor may be operated SSF with cellulase enzyme to clean up the hydrolyzed oligosaccharide fragments. Again, ethanol and CO 2 can be efficiently vacuum evaporative extracted from the fermenters.
  • the use of the robust bacterium Zymomonas mobilis, genetically engineered to ferment five-carbon sugars as well as glucose, and the yeast Saccharomyces cervisiae support rapid fermentation of all the five- and six- carbon sugars liberated in the two cellulosic hydrolysis steps.
  • Concentrating the substrate sugars to order 20%> in aqueous solution and retaining order 20% biocatalyst loading against the substrate with a comparatively low dilution water volumetric exchange rate of order 0.1 per hour will realize mean fermentation volume utilization in about one day, efficiently matching the performance of the enzymatic hydrolysis step.
  • a major objective of the invention is to build broad flexibility into the present process with regard to value adding product diversity, while maintaining energy efficiency and clean, functional consistency in the face of the fact that many chemical products and coproducts of interest, such as the volatile organic components of the Stage 1 hydrolysate, will have boiling points greater than that of water. Accordingly, the same product recovery, including fractional distillation and possibly solvent extraction are applied here as were described above with reference to Embodiment 1. The same economic, energy and environmentally sound practices discussed with reference to Embodiment 1 are also preferably applied here.
  • the tests in question involve two-stage dilute acid hydrolysis by Brink using nitric acid and single-stage dilute acid hydrolysis of Nguyen using sulfuric acid. Both acids are similarly efficacious from a hydrolysis standpoint.
  • the two-stage approach is founded in the understanding first that hemicellulose is more readily hydrolyzed under milder conditions of pressure, temperature and acid concentration than cellulose. Second, glucose (derived principally from cellulose) is more resistant to chemical degradation after depolymerization than xylose, the principal product of hemicellulose.
  • Nguyen has provided the analysis of chemical composition of (the representative) mixed feedstock in wt%:
  • VOCs AC, acetic acid; FF, furfural; HMF, hydroxymethylfurfural
  • cellulases are in fact well known combinations of enzymes that work by attaching polysaccharide chains both in mid-chain and near the ends, they do their work inherently by repetitively fractionating the polymeric chemicals and ultimately their oligosaccharide fragment products.
  • One advantage of a process in accordance with the present invention which uses two-stage dilute acid hydrolysis followed by enzymatic hydrolysis is that most of the work of breaking up the cellulosic chains is more easily accomplished by the acid, giving the enzyme an open field to polish off the uncompleted work at low cost in catalyst and facilities in conjunction with the simple SSF oligosaccharide/yeast fermentation reactor.
  • Embodiment 1 because the volume of material to be enzymatically digested in Embodiment 1 is reduced by an order of magnitude relative to Embodiment 2, similar reductions in the volume of costly enzyme and, most importantly, large reductions in dilution water needed to control end-product inhibition, are possible.
  • the latter problem with heretofore brute-force enzymatic hydrolysis i.e., without second-stage acid prehydrolysis is extensively discussed Lombard (reference 10).
  • the dilution water problem which can require massive volumes of filtration, is here further obviated by the use of SSF (simultaneous saccharification and fermentation) in processes in accordance with one embodiment of the present invention to remove competing sugars from the reactor by fermentation in pace with their production by enzymatic hydrolysis.
  • SSF simultaneous saccharification and fermentation
  • the sugars are both generated by acid hydrolysis and efficiently fermented over nominally a day in the bacterial system, leaving only about 10% of the problem for the SSF reactor.
  • the SSF recycle reactor with easily hydrolysable oligosaccharides and concentrated yeast and enzyme catalyst, can be given all the performance desired at very modest cost in infrastructure and overhead.

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Abstract

La présente invention concerne des procédés et des systèmes de production de produits organiques utiles à partir de biomasses diverses contenant de la lignocellulose qui présentent un rendement élevé par rapport aux procédés existants. Particulièrement, cette invention combine les techniques de délignification alcalines et d'hydrolyse d'acide dilué dans des procédés pour améliorer le rendement et l'efficacité du traitement de la biomasse lignocellulosique et permettre la production économique de plastiques biodégradables à base de lignine et d'autres produits organiques.
PCT/US2000/030438 1999-11-02 2000-11-02 Procede de production de produits organiques a partir de sources de biomasses diverses contenant de la lignocellulose WO2001032715A1 (fr)

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