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    • 专利摘要:
    method and system for fractioning lignocellulosic biomass methods and systems for fractioning lignocellulosic biomass that includes hemicellulose, cellulose and lignin, which includes blowing up biomass cells to de-decolactize biomass, hydrolyze hemicellulose to produce a liquid component that includes hemicellulose sugars and a liquid component solid component that includes less than 10% hemicellulose, separate the liquid and solid components, vaporize the cellulose into the solid component, and condense the cellulosic sugar values. the methods and systems can vaporize cellulose in a continuous steam reactor at a temperature of about 400 to 550 <198> c and a pressure of about 100 to 300 kpa (1 to 3 bara). electromagnetic and / or electroacoustic treatment such as ultrasound and / or microwave treatment can be applied to biomass just before or during cellulose hydrolysis.
    公开号:BR112012007026B1
    申请号:R112012007026-6
    申请日:2010-09-29
    公开日:2020-01-07
    发明作者:Peter Herbert North
    申请人:Nova Pangaea Technologies Limited；
    IPC主号:
    专利说明:

    METHOD AND SYSTEM FOR BIOMASS FRACTIONATION
    LIGNOCELLULOSIS
    PRIORITY This patent application claims priority over Provisional Patent Application serial number U.S. 61 / 246,721, filed on September 29, 2009, the disclosure of which in its entirety is hereby incorporated by reference in its entirety for reference.
    BACKGROUND
    It is generally accepted that fossil fuels are both limited as a resource and also cause a network to increase in global emissions of carbon dioxide, a greenhouse gas involved in a potential global warming scenario. These fossil fuels, in particular oil, are essential for the production of liquid transport fuels and the vast majority of chemicals, in addition to providing a significant proportion of static energy generation.
    The only significant alternative source for liquid transport fuels and chemicals is biomass, like lignocellulosic biomass, and considerable effort has been put into it for many decades to produce economical and efficient processes for converting biomass to form such fuels and chemicals.
    Woody or lignocellulosic biomass is largely composed of hemicellulose, cellulose and lignin. Sources of lignocellulosic biomass include wood and wood waste, agricultural waste such as corn straw, woody grasses and residential and industrial waste. Each of the main components of lignocellulosic biomass is a valuable material. For example, cellulose mainly comprises C6 sugars (glucose) which can be further processed to produce ethanol, a commercial fuel, or coated as an anhydrous sugar, levoglucosan, or as levulinic acid and fine chemicals, mixed higher alcohols and most valuable fuels. Hemicellulose comprises C5 or C6 sugars such as xylose, arabinose, galactose, glucose and mannose. These sugars can also be fermented with ethanol or covered as furfural and other derivatives and further processed into fine chemicals, alcohols and other commercial fuels. Lignin is a complex polymer that can be further processed into fine chemicals (such as phenol and fuel additives) or can be used as a direct fuel for generating heat and power for processing and export.
    The lignin component of lignocellulosic biomass materials gives physical strength to the biomass and is firmly linked to the cellulose and hemicellulose components. Therefore, although it is desirable to fractionate the biomass, the presence of lignin makes fractionation difficult, and the severe conditions required for fractionation can result in the breakdown of carbohydrates in less desirable products.
    Various methods have been tried to remove sugars from carbohydrates present in hemicellulose and cellulose from biomass. For example, chemical and biochemical processes that use enzymes, solvents, acid, alkali-based, or hot water can be used to try to dissolve the lignin or carbohydrate components of the lignocellulosic biomass with or without concomitant hydrolysis. In addition, various forms of pre-treatment, such as acid or alkali processes, explosion of water vapor and hot water, try to make carbohydrates accessible for separation. However, separating biomass into fractions and isolating each of these fractions, while avoiding the production of by-products and minimizing energy consumption (and therefore the cost of production) remains difficult.
    The processes revealed so far for the conversion of biomass into fuel can, in general, be considered included in one or the other between the following two categories. A category is a thermochemical treatment of the entire biomass, without fractioning or separating the component parts of the biomass, by means of pyrolysis, gasification or liquefaction, which generates, in the first place, a mixture of synthesis gas or crude bio-oil. The other category includes physical and chemical pretreatments of the entire biomass, destined for the destruction or neutralization (instead of separation and collection) of the volatile or extractable components and the hemicellulosic components of the biomass (which would otherwise inhibit the stage or subsequent conversion steps), followed by a chemical or microbiological (enzymatic) hydrolysis of the cellulosic components and a microbiological fermentation of the resulting cellulosic sugars. Other processes are also known to be, in general, of a chemical nature and performed in the liquid phase, such as dissolution and solvent separation of one or more of the main components, including supercritical extraction processes.
    All of these processes are, in general, directed towards the production of liquid transport fuel or the production of a specific chemical or range of chemicals or products such as fiber board.
    summary
    The modalities of the inventions described in this document include systems, methods and devices for the fractionation of lignocellulosic biomass. This fractionation can be used for the recovery and isolation of hemicellulosic and cellulosic sugars including C5 and C6 sugars, lignin, and / or other biomass components. This fractionation can be carried out using continuous processes, such as one or more continuous water vapor tubes, which allow quick and effective separation of the biomass components.
    Some embodiments of the present invention provide improved thermochemical processing functionality. Some systems receive crude biomass as input intake and produce hemicellulosic sugars, cellulosic sugars and relatively pure lignin as a product. Some systems receive relatively pure hemicellulose solids as a product and produce sugars isolated from relatively pure lignin-cellulose solids and hemicellulose as products. Some systems receive relatively pure lignin-cellulose solids as a product and produce sugars isolated from lignin-cellulose charcoal. In some systems, one, two, or all three systems discussed in this paragraph can be included as subsystems. Any of the systems discussed in this paragraph can be implemented as continuous flow processes.
    In some embodiments, the invention includes a method of fractioning and treating lignocellulosic biomass material that includes first, second and third water vapor reactors. The method includes preparing the biomass by reducing its size, treating the biomass using superheated water vapor and / or EM / EA treatments, and feeding the treated biomass into a first continuous superheated steam cycle reactor to separate and hydrolyze hemicellulose and produce a solid and liquid component. The liquid component includes hemicellulose hydrolyzed in water or an aqueous solvent mixture and is separated from the solid component. The method additionally includes optionally feeding the biomass in a second continuous superheated steam cycle reactor to reduce the water content of the biomass and / or to recover energy, feeding the solid component into a third continuous superheated steam reactor (for example, a tube) to separate and hydrolyze the cellulose component and to volatilize the products forming the water vapor vapor and to separate it from a lignin charcoal, and condensing the water vapor and hydrolyzed cellulose.
    In some embodiments, the invention includes a method for fractionating lignocellulosic biomass material that includes feeding the biomass in a devolatilization reactor to separate and collect volatile components from the biomass, feeding the biomass in a hemicellulose hydrolysis reactor to separate and hydrolyze the hemicellulose , separate the biomass into a first solid component and a liquid component, where the liquid component includes hemicellulose hydrolyzed in water or solvent and where the solid component includes cellulose and lignin and has less than about 10% hemicellulose, feed the 5 solid component in a cellulose hydrolysis reactor that comprises a continuous superheated water vapor reactor to hydrolyze and vaporize the cellulose component, and to condense the vaporized cellulose. In some embodiments, the cellulose hydrolysis reactor applies water vapor to the biomass at a temperature of at least 300 2 C. In some embodiments, the cellulose hydrolysis reactor applies water vapor to the biomass at a temperature between about 400 and 550 a C. The cellulose hydrolysis reactor can apply pressure to the biomass in 100 to 3 00 KPa. In some 15 modalities, the cellulose hydrolysis reactor applies water vapor to the biomass at a temperature of between 400 and 550 2 C and at a pressure of 100 to 300 KPa (1 to 3 bara).
    In some embodiments, the invention includes a method of isolating cellulose from a biomass that includes feeding a biomass into a cellulose hydrolysis reactor, the biomass includes lignin and cellulose and less than about 10% hemicellulose, hydrolyzing and vaporizing a portion of the cellulose in the cellulose hydrolysis reactor, separate the vaporized cellulose from a remaining biomass solid 25, and condense the vaporized cellulose. In some embodiments, the method additionally includes feeding the biomass in a hemicellulose hydrolysis reactor to separate and hydrolyze the hemicellulose before feeding the biomass in the cellulose hydrolysis reactor. In such 30 embodiments, the method additionally includes separating the biomass into a first solid component and a liquid component, wherein the liquid component includes hemicellulose hydrolyzed in water or solvent, where the solid component includes cellulose and lignin in less than 10% of hemicellulose, and where the step of feeding a biomass in a cellulose hydrolysis reactor includes feeding the solid component in the cellulose hydrolysis reactor.
    A cellulose hydrolysis reactor can apply only water vapor to the biomass solid or it can apply a mixture of water vapor and another gas. For example, the reactor can apply a mixture of water vapor and nitrogen, hydrogen, carbon dioxide, carbon monoxide or combinations of more than one gas.
    The cellulose hydrolysis reactor can also apply electromagnetic or electroacoustic treatment (EM / EA) to the biomass. For example, the cellulose hydrolysis reactor can apply Pulsed Electric Field, ultrasonic energy, microwave energy or combinations of these to biomass in the reactor. In some modalities, the cellulose hydrolysis reactor applies ultrasonic energy to the biomass, while in other modalities, it applies microwave energy to the biomass, while in still other modalities, it applies both ultrasonic and microwave energy to the biomass. biomass.
    After hemicellulose hydrolysis and before feeding the biomass into the cellulose hydrolysis reactor, the methods of the invention can feed the solid component of the biomass in a dryer to reduce the water content of the solid component. In some embodiments, the dryer is a continuous superheated water vapor cycle reactor. In some embodiments, the methods of the invention may include friction of the solid component after removing it from the reactor for hemicellulose hydrolysis and before feeding the solid component into the reactor for cellulose hydrolysis. For example, the methods of the invention may include, first, drying the biomass and then friction of the biomass before cellulose hydrolysis.
    The cellulose hydrolysis reactor can completely hydrolyze the cellulose to produce a vapor of cellulosic sugars and a lignin coal. The cellulose hydrolysis reactor can produce a vapor of cellulosic sugars and a second solid component. The second solid component can be fed into a second reactor, which can be an overheated water vapor reactor. In some embodiments, the cellulose hydrolysis reactor partially hydrolyzes cellulose, and the second reactor is a second cellulose hydrolysis reactor that completes cellulose hydrolysis and separates vaporized cellulosic sugar from lignin. In other embodiments, the cellulose hydrolysis reactor completes the cellulose hydrolysis and the second reactor reduces lignin to a condensable gas that can be recovered.
    The embodiments of the invention also include systems for the fractionation of cellulosic biomass material including a means to release volatile components from biomass, a means to hydrolyze hemicellulose into biomass, a means to separate the biomass into a solid component and a liquid component in which the liquid component includes hydrolyzed hemicellulosic sugars, and a means to hydrolyze and vaporize cellulose. The system may further include a means for drying the solid component of the biomass after separation of the solid component and the liquid component. In some such embodiments, the system may further include an attritor for the friction of the solid component after drying. In some embodiments, the means for hydrolyzing and vaporizing cellulose includes an electromagnetic or electroacoustic generator to apply electromagnetic or electroacoustic treatment to biomass.
    In some modalities, the method includes preparing a lignocellulosic biomass material that has intact cells for fractionation which includes supplying the biomass, feeding the biomass in a superheated water vapor reactor at high pressure, heating the biomass with water vapor overheated while the high pressure is maintained to explode the biomass cells inside the water vapor reactor, and separate the exploded biomass from the water vapor. In some embodiments, heating includes heating the biomass to a temperature between about 150 ° C and about 190 ° C in about 5 to about 10 seconds. In some embodiments, the temperature of the biomass is increased to between about 150 ° C to about 190 ° C and the pressure is maintained at about 1000 to about 1500 kPas. In some embodiments, the superheated water vapor reactor comprises a tubular structure in which the water vapor circulates continuously in a cycle. In some of these modalities, biomass flows through the reactor while being dragged through water vapor. In some embodiments, the method additionally includes applying EM / EA treatment to the biomass inside the reactor. EM / EA treatment can include microwave, ultrasound, pulsed electric field, or a combination thereof.
    In some embodiments, the method of preparing a lignocellulosic biomass material that has the cells intact for fractionation includes additionally releasing the volatile components of the biomass into the water vapor. The method may also include separating the volatile components from the water vapor.
    In some embodiments, the method of preparing a lignocellulosic biomass material that has intact cells for fractionation also includes feeding the biomass exploded in the hemicellulose hydrolysis reactor to hydrolyze the hemicellulose, separating the biomass into a solid component and a liquid component in which the liquid component includes the hydrolyzed hemicellulose and in which the solid component includes cellulose and lignin, and the feeding of the solid component into a cellulose hydrolysis reactor to hydrolyze the cellulose component and separate the cellulosic sugars from the lignin. The hemicellulose hydrolysis reactor and / or the cellulose hydrolysis reactor can be a continuous superheated water vapor reactor.
    The modalities of the invention also include systems for preparing a lignocellulosic biomass material that has the cells intact for fractionation which includes a tubular water vapor reactor, a water vapor inlet to enter the superheated water vapor into the reactor of water vapor, a blower to continuously move water vapor through the reactor, a biomass inlet in the water vapor reactor to enter the biomass material, and a biomass outlet into the steam reactor water and downstream of the biomass inlet to remove the biomass, where the reactor is designed to maintain the water vapor at a temperature and pressure sufficient to rupture or explode the biomass cells as the biomass passes between the biomass inlet and the outflow of biomass. For example, the temperature can be from about 150 ° C to about 190 ° C and the pressure can be from about 1000 to about 1500 kPas. The blower can be designed to circulate the water vapor at a speed sufficient for the biomass to be drawn into the water vapor and to pass from the entrance to the exit in about 5 to about 10 seconds. In some embodiments, the reactor comprises a water vapor cycle in which water vapor circulates continuously through the cycle. The system may additionally include an outlet to separate and remove volatile components from the biomass released by the explosion of the biomass cells.
    The system for preparing a lignocellulosic biomass material that has intact cells for fractionation can also include an EM / EA treatment source between the biomass inlet and outlet, such as a microwave, ultrasound, pulsed electric field generator, or a combination of them.
    Modalities of the invention also include methods of fractioning lignocellulosic biomass material which includes feeding the biomass in a devolatilization reactor, feeding the biomass prepared in a hemicellulose hydrolysis reactor to separate and hydrolyze hemicellulose, separating the biomass into a solid component and a component liquid where the liquid component includes hemicellulose hydrolyzed in water or solvent and where the solid component includes cellulose and lignin, feed the solid component into a cellulose hydrolysis reactor to hydrolyze the cellulose component, and separate the hydrolyzed cellulose from lignin, in which the EM / EA treatment is applied to biomass in the devolatilization reactor, to the hydrolysis of hemicellulose reactor, and / or in the cellulose hydrolysis reactor. EM / EA treatment can include microwaves, ultrasonic energy, pulsed electric field, or a combination of them. Reactions in the reactors can be increased, supplemented, or interspersed with the use of EM / EA treatment.
    In some modalities, the EM / EA treatment is applied to biomass both in the hemicellulose hydrolysis reactor and in the cellulose hydrolysis reactor. In some modalities, EM / EA treatment is applied to a parameter that includes frequency, shape, power or pulse duration, and one or more of these parameters is adjustable. EM / EAs treatment can assist in cell disruption (lysis), especially at low temperatures, in increasing the rate of heat transfer through cell aggregates, increasing permeability of cell membrane, degrading or reducing polymeric structures of hemicellulose, cellulose and lignin, assist in hydrolytic and other reactions of carbohydrate polymers, and assist in the extraction of lipids, proteins and non-carbohydrate components from cells.
    In some embodiments, the hemicellulose hydrolysis reactor is a recirculating tube reactor. In some embodiments, the hemicellulose hydrolysis reactor is a tube reactor.
    In some embodiments, the devolatilization reactor comprises a superheated water vapor reactor at high pressure that quickly heats the biomass with superheated water vapor while maintaining high pressure to explode the biomass inside the water vapor reactor. In some such modalities, the EM / EA treatment is applied to the biomass inside the devolatilization reactor. The method can also include releasing, separating, and removing volatile components from biomass in the devolatilization reactor.
    In some embodiments, a biomass fractionation system includes means to release volatile components from biomass, means to hydrolyze hemicellulose in the biomass, means to hydrolyze and vaporize cellulose, and an EM / EA generator to apply EM / EA treatment to the biomass in one or more of the above means.
    In some embodiments, the invention includes a system for fractionating lignocellulosic biomass material that comprises a first superheated water vapor cycle reactor to explode biomass in the water vapor cycle, a second water vapor cycle reactor superheated to hydrolyze hemicellulose, a third superheated water vapor cycle reactor to reduce the moisture content of the biomass and a fourth superheated water vapor reactor to hydrolyze cellulose in a water vapor and form a lignin coal , in which the biomass is continuously transported through the first, second, third and fourth water vapor reactors.
    In some embodiments, the hemicellulose hydrolysis step employs two or more stages of continuous processing. In some embodiments, the hemicellulose hydrolysis step includes moving the biomass to a screw, extrusion or other transport system to continue hemicellulose hydrolysis. The hydrolyzed hemicellulose can be extracted using sequential multi-step washing, with water or water / solvent mixtures, and remove water at high pressures. Alternatively, the hydrolyzed hemicellulose can be extracted by passing the biomass to a pressure of about 100-200 bars and pouring with water or water / solvent mixtures. In some modalities, hydrolyzed hemicellulose has the water removed by applying a high pressure screw or extrusion presses to biomass. In some embodiments, residual biomass solids include cellulose and lignin and less than 10% hemicellulose. Residual solids can then undergo friction.
    In some modalities, energy is recovered in the form of high pressure water vapor, part or all of which is superheated, such as the water vapor that carries it to the cellulose hydrolysis stage.
    Brief description of the Figures
    The following drawings are illustrative of particular embodiments of the present invention and, therefore, do not limit the scope of the invention. The drawings are not to scale (unless stated) and are intended for use in conjunction with the explanations in the following detailed description. The modalities of the present invention will hereinafter be described together with the accompanying drawings, in which similar numbers denote similar elements.
    Figure 1 is a schematic diagram of a system for preparing lignocellulosic material for fractionation;
    Figure 2 is a schematic diagram of an alternative system for the preparation of lignocellulosic material for fractionation;
    Figure 3 is a schematic diagram of a devolatization system;
    Figure 4 is a schematic diagram of a continuous flow water vapor cycle reactor for the hydrolysis and fractionation of hemicellulose;
    Figure 5 is a schematic diagram of another modality of a continuous flow water vapor cycle reactor for the hydrolysis and fractionation of hemicellulose;
    Figure 6 is a schematic diagram of an alternative modality of a continuous flow water vapor cycle reactor for the hydrolysis and fractionation of hemicellulose;
    Figure 7 is a schematic diagram of another alternative modality of a continuous flow water vapor cycle reactor for the hydrolysis and fractionation of hemicellulose;
    Figure 8 is a schematic diagram of a continuous flow rapid thermolysis system for cellulose hydrolysis and cellulose and lignin fractionation;
    Figure 9 is a schematic diagram of an alternative continuous flow thermolysis system for cellulose hydrolysis and cellulose and lignin fractionation; and
    Figure 10 is a flow chart of a biomass fractionation process.
    description
    The following detailed description is exemplary in nature and is not intended to limit the scope, applicability or configuration of the invention in any way. In particular, the following description provides practical illustrations for implementing exemplary embodiments of the present invention. Examples of constructions, materials, dimensions, and manufacturing processes are provided for selected elements, and all other elements employ what is known to elements skilled in the art of the invention. Elements skilled in the art will recognize that many of the examples provided have suitable alternatives that can be used.
    Modalities of the invention can be used to provide a complete fractionation of biomass in all its constituent parts (such as volatile / extractable; hemicellulose sugars; cellulosic sugar; lignin phenols; proteins; inorganic salts; etc.), while maintaining as much as possible the structural complexity of the individual monomeric chemical constituents. Thus allowing a very wide range of liquid and chemical transport fuel products to be produced in a flexible and economical way. From these primary products, many of which are platform chemicals, the complete complexity of today's organic chemicals industry can be recreated. The bio-oil produced is both less complex and less difficult, since it is primarily a product of cellulosic hydrolysis and depolymerization, with a much smaller contribution from other components, as compared to other processes.
    In addition, modalities of the invention can be designed to provide a low, continuous resistance time, a vapor phase process that is then capable of extending to very large scales (such as 50,000 to 500,000 barrels of oil equivalent per day) in one single site. This ensures economies of scale and is compatible with the scale of oil refineries. The fuel products can then be produced on a scale commensurate with the current global oil demand of 80 million barrels per day and secondary processing, in a bio-refinery complex, which may be of an equivalent current chemical industry scale.
    Modalities of the invention may also include the application of technologies not generally found in other processes. These technologies can be used to improve heating and mass transfer to and from solid biomass particles, which are generally limited in other processes and define restrictions on their capacities, thus leading to increased yields and reaction and residence times. reduced.
    As such, the embodiments of the invention can provide the primary component of an integrated bio-refinery, which generates platform chemicals and fuel-based stocks suitable for further chemical synthesis or refinement, as appropriate.
    Methods and systems of the invention include systems and processes for fractionating lignocellulosic biomass into monomeric and oligomeric components that include C5 sugars and derivatives, C6 sugars and derivatives, lignin and other lower components. In some modalities, some or all of the fractionation processes use a continuous flow process, making it possible to fractionate very large amounts of biomass with high efficiency and reduced cost.
    Biomass is primarily prepared for fractionation. This preparation involves the standard operations normally involved for the specific biomass used (cleaning, etc.) and may include reducing the size of the biomass, de-aerating the biomass, and / or pre-heating the biomass. This can also include the extraction of valuable components like amino acids or oils. The biomass is then opened by some means of cell disruption, such as steam explosion. In some embodiments, the steam explosion uses a process of rapidly heating the biomass in a continuous steam loop reactor under increased pressure, exploding the biomass cells and removing the volatile components of the biomass. In other modalities, the steam explosion can be supplemented, multiplied or replaced by EM / EA treatments.
    After preparation, extraction and devolatilization of the biomass, it is then subjected to hemicellulose hydrolysis. In some embodiments, hemicellulose hydrolysis includes a two-stage process that includes a first high-pressure steam loop stage to initiate hydrolysis, followed by a second stage of the retention system as a conveyor belt system to complete the process of hemicellulose hydrolysis. In other embodiments, the first stage of hemicellulose hydrolysis may include more than one high pressure steam treatment, followed by a second stage of retention system. The hydrolyzed hemicellulose dissolves in an aqueous solution and is separated from the remaining biomass solid by a leaching system.
    The biomass solid can then be dried to a desired moisture content and can be broken down to a fine particle size. However, in some modalities, such as modalities that employ EM / EA treatments during cellulose hydrolysis, drying and crushing may not be included. The next step is cellulose hydrolysis. In some embodiments, cellulose hydrolysis includes rapid thermolysis. Rapid thermolysis can be performed in a continuous steam reactor under low temperature and pressure, such as between about 350 and about 450 degrees Celsius. Under these conditions, the bond between the lignin and the cellulose is broken and the hydrolyzed cellulose can be removed in a vapor stream with steam while the lignin forms a solid coal. In some embodiments, cellulose hydrolysis is performed in two or more stages using two or more superheated steam reactors, with each subsequent reactor at a higher temperature than each previous reactor.
    The methods and systems of the invention can be performed using continuous systems such as continuous steam reactor (for example, loops, tubes, etc.) and conveyor systems, for example, allowing for a continuous processing system. As such, this avoids the time delays inherent in systems that use batch processing. The continuous processing systems described in this document are also more energy efficient than batch systems, because they do not require repeatedly increasing pressure or temperature for each batch, but in particular, steam reactors should only maintain the desired pressure and temperature as required. biomass materials enter and flow through the systems. Inherent control accuracy allows for a gradual increase in treatment severity and results in a complete and complex fractionation of the biomass.
    Preparation of lignocellulosic material
    The biomass fractionation process begins with the preparation of the biomass material. Modalities of the invention can use any lignocellulosic material, such as soft or rigid wood, grasses, agricultural waste, other plant material, urban waste, or a combination of one or more biomass materials. Examples of wood useful in embodiments of the invention include pine, poplar, fir, pine, larch, beech, oak, and palm and palm scraps, for example. The material may include logs, stems, branches, roots, heartwood, wood scraps, wood bark, sawdust, wood pruning and forest waste, for example. Agricultural material or refuse that can be used in embodiments of the invention includes corn husks, corn cobs, corn seeds, corn fibers, straw, banana plantation refuse, rice straw, rice husks, oat straw, husks oat, corn fiber, cotton stalk, cottonseed, wheat straw, sugar cane bagasse, sugar cane disposal, sorghum waste, sugar processing waste, barley straw, grain straw, straw wheat, canola straw, and soy straw, for example. Grasses can include yellow millet, esparto, ryegrass, miscantus, Bermuda grass, capimamarelo and alfalfa. Other plant materials may include wood material and plant wood which includes logs, stems, shrubs, foliage, bark, roots, cocoons, nuts, skins, fibers, vines, and algae. Urban waste may include residential waste such as waste paper and food and industrial waste such as paper and board waste, paper mill sludge and other cellulosic waste.
    Biomass can be introduced into a storage preparation system or direct from transit. It can first be passed through the cutting pouch or other automated decontamination process, if required, and then to a metal detection and removal process and / or a pressure or other washing process, in which dirt and stones are removed from the biomass.
    The biomass can then be conducted and processed in a drying system, such as an air jet or other
    system in drying, to remove the excess water gives surface. Clean biomass can then be passed on one or more crushing stages. 0 lignocellulosic material submit The
    crushing, as for creating chips or flakes, to achieve a desired particle size. This can be done by a sieving and peeling machine, a knife ring crusher with vibrating protection, for example. The particle size is chosen so as to keep the biomass in suspension and allow heat transfer through the biomass in the continuous reactor system, which depends on vapor velocity, biomass density, and biomass format, among other similar factors. In some embodiments, the material is teased from about 0.5 to 5 mm in thickness and about 12 to 80 mm in width and height. The preferred particle size may depend on the diameter of the tubes used in the subsequent processing steps. Some modalities crush material of about 0.5 to 1.5 mm in thickness and about 12 to 15 mm in width and height. Some modalities crush material of about 2 to 5 mm in thickness and about 60 to 80 mm in width and height. The preferred size of flakes measures about 1 to 3 mm in thickness, and about 25 to 40 mm in height and width in some embodiments. Preferred material sizes can also be expressed in terms of equivalent spherical particle diameters. Consequently, preferred sizes can be about 5 to 10 mm in equivalent diameter. In some embodiments that have cylindrical sections, such as grass-type raw materials, preferred sizes can be about 2 to 5 mm in diameter and 25 to 50 mm in height. The particle size is a function of the capacity of systems and, therefore, dimensions as well as characteristics of raw material, so that some modalities can employ other ranges of size.
    Some material can be determined by a sieve, to be undersized. In some embodiments, the proportion of undersized material can be added to the material of the desired size for further processing, with the rest being passed to different processing systems. In some cases, a different processing system may be a system for fractionating biomass, with the size of the system being configured to handle smaller material sizes (for example, a smaller capacity, smaller diameter loop system). Too large material can be recycled to the flaking or shredding machine and teased to the desired size. It is expected that a commercial system can have a number of reactor systems that operate in parallel, with each system processing biomass material of a different size and / or different raw material.
    In some embodiments, the biomass starting material can be comprised of many different materials, such as tree bark, branches, and leaves. Processing such material to reduce its size also makes the material more homogeneous and thus more suitable for processing. At the desired thickness, as described above, heating transfer to the biomass center occurs quickly enough, creating a useful size for use in the steam reactor processes described below. In addition, the use of long, thin pieces like flakes, for example, allows pieces thin enough for rapid heating, but is still large enough to allow cyclonic separation of solid biomass from steam, as in a cyclonic separator, as can occur in several stages of the fractionation processes described in this document. In some embodiments, the process of reducing material size (for example, by feeding, grinding, and sifting) takes approximately one minute.
    In some embodiments, the lignocellulosic material can be further processed to remove air from the biomass. This can be achieved by applying a vacuum to the biomass and / or replacing air in the biomass with an inert gas such as CO 2 or nitrogen. In some modalities, subsequent stages of the fractionation process produce CO 2 that can be collected and used to de-aerate the biomass starting material. In some embodiments, the biomass material is installed under a vacuum or partial vacuum and an inert gas is released into the material, replacing the air and removing oxygen from the material. The removal of oxygen from the material is desirable to reduce the level of oxidative degradation of products and other undesirable reaction mechanisms, which can occur increasingly at elevated temperatures and pressures and in the presence of acid catalysts. The yield of sugars and other preferred products can be reduced by oxidative degradation, leading to reduced yields of fuel and other by-products. Degradation can also generate gaseous products, such as CO 2 , which can result in raw material waste.
    The preparation of the lignocellulosic material can optionally include the removal and collection of volatile and other non-lignocellulosic components such as essential oils, terpenes, amino acids, etc. where these components exist in significant proportions and have commercial value. For example, eucalyptus oil can be removed and isolated before fractioning eucalyptus wood to extract the maximum value from the raw material. Proteins and amino acids can be removed from grass and crop waste, for use in animal feed or pharmaceutical products. These components can be recovered to be of commercial value and / or to avoid interference in the fractionation process or contamination of fractionation products. They can be removed using a completely continuous process. In some embodiments, these components are removed through one or more extraction steps. In some embodiments, the extraction steps comprise a continuous countercurrent extraction process using one or more solvents. The extraction step can use one or more EM / EA treatments such as pulsed electric fields (PEF), ultrasonic energy (US) and / or microwave (MW) to smooth cells and to carry out mass transfer of the components of interest in the solvents . EM / EA treatments can be applied to biomass or just before or during extraction. These extractions can be done at room temperature or at a high temperature, such as a temperature between room and approximately 150 degrees Celsius, or between about 60 and about 120 degrees Celsius. Solvents can be chosen based on the type of soluble component to be extracted. Examples of suitable solvents include hydrocarbons, such as mineral oil, ketones, alcohols and / or aromatics. In some embodiments, a first solvent is applied to the biomass material and the soluble component or components are removed from the material by pouring the solvent through the material, collecting the solvent, and isolating or separating the soluble component. A second solvent is then applied to the material to allow the first solvent to be washed using a subsequent water wash. The second solvent can also be collected and the soluble component and / or first solvent can be separated from the second solvent and isolated. For example, the second solvent can be either hydrophilic or hydrophobic so that it is able to dissolve the first solvent and can then be washed with the subsequent water wash. One or more water washes can then occur through the material. In some embodiments, such extraction steps can take approximately two and a half minutes, with each step taking approximately one minute plus approximately 30 seconds for total feeding and unloading.
    The extraction stage of volatile and other non-lignocellulosic components can be performed by countercurrent or concurrent continuous extraction equipment, such as a single or double screw extruder or belt conveyor, a vertical flat extractor, a rotary extractor, or a centrifugal extractor , for example.
    In some embodiments, the optional removal of volatile and other non-lignocellulosic components can be provided as a side flow. In such embodiments, the part of a biomass for such extraction that is desired can be diverted to a lateral flow, such as a series of countercurrent extractions as described above. The flow to the lateral extraction flow can then be interrupted and the biomass flow without extraction can proceed directly to the preheating step or to the hemicellulose hydrolysis reactor. In such embodiments, the biomass flow from a preparation stage includes a branch for optional extraction or to bypass extraction. Such systems allow flexibility in treating various biomass materials so that extraction may or may not be desired.
    The lignocellulosic material can be further processed by preheating the material. For example, the material can be preheated using active steam (ie steam injected directly into the process), hot solvent or indirect heating. For example, in some embodiments, the material can be preheated using low pressure steam. In some embodiments, low pressure steam can be applied to the material using a continuous process so as to include a belt conveyor, such as a screw conveyor. The material can be preheated to a temperature between approximately 100 and approximately 200 degrees Celsius, as a temperature between approximately 120 and approximately 150 degrees Celsius. The material is preheated to reduce thermal demand in the first steam reactor and to ensure that the reactor operating temperature is quickly reached. The temperature is preferably maintained below which significant hemicellulose hydrolysis occurs, such as less than 180 degrees Celsius. In some modalities, the biomass deaeration and preheating process can take approximately two to three minutes.
    In some embodiments, the process for removing the non-lignocellulosic components previously described is a hot solvent extraction process. In such a process, one or more of the solvents are at an increasing temperature when applied, resulting in heating of the biomass. The hot solvents can thus perform the function of preheating the biomass to a desired temperature as well as extraction.
    In some embodiments, a water content adjustment step can be included to bring the water content of the biomass to the desired level. For example, it may be necessary to add water to dry biomass like straw. The water can be added as steam or water during a preheating step as described above. Alternatively, water can be added to the devolatilization reactor to supplement the water released from the biomass, to maintain the required superheated steam flow rate. For example, the water content can be increased to about 50%.
    Modalities of systems for the preparation of a lignocellulosic biomass material for fractionation are shown in Figures 1 and 2. A lignocellulosic biomass material is fed from the storage of raw material in a sieving and flaking machine 2 to reduce the raw material to a desired size. The raw material is then passed through an inlet of the de-aeration system 4 and then into a de-aeration system 6 that removes the air from the biomass using a vacuum 8. The vacuum is broken (or the displaced air) with an inert gas (N 2 or CO 2 ). Deaeration system 6 includes a belt conveyor, such as a screw conveyor, which transports biomass out of the deaeration system through which the biomass exits the deaeration system
    6.
    In the system shown in Figure 1, the biomass then passes through a first, second, and third solvent washing system 12, 14, 16, each of which includes an inlet 18, 20, 22 and an outlet 24, 26, 28, although alternative modalities could include more or less than washing systems. In each solvent washing system 12, 14, 16, biomass enters through inlet 18, 20, 22, and is conducted through system 12, 14, 16 on or in a continuous processing unit such as a conveyor belt conveyor. screw, and exit through outlet 24, 26, 2 8 to proceed to the next step in the process. The solvent washing systems 12, 14, 16 as shown, are each countercurrent washing system. The first solvent washing system 12 uses a first solvent, and can also be equipped with one or more systems that employ one or more of the EM / EA 2 9 treatment generators (such as PEF, US, MW) that open the cells and accentuate the extraction of the components of interest in the solvent. The second solvent washing system 14 uses a second solvent. The soluble component dissolved in each solvent is recovered from each solvent wash after passing or spilling through the biomass. The solvents can then be reused for additional solvent washes. After the two solvent washes, the biomass is washed in the third solvent washing system 16 with hot water, again using a counterflow system. In some embodiments, the water is at a temperature between about 90 and about 200 degrees Celsius. In other modalities, the water is at a temperature between about 120 and about 150 degrees Celsius. The solvent is removed from the biomass by hot water, while at the same time, the hot water preheats the biomass to the desired temperature before the biomass moves on to the next stage of the fractionation process. In some modalities, the next stage is the devolatilization of biomass.
    An alternative biomass preparation system is shown in Figure 2. In this system, there is no solvent washing and as such, it can be used when there is no valuable extract. However, the system can still employ a hot water wash 16 as described with respect to Figure 1. In such embodiments, the hot water wash 16 works to preheat the biomass before further processing.
    It must be recognized that the systems shown in Figures 1 and 2 can represent two distinct systems. Alternatively, a system can include both the process shown in Figure 1 and the process in Figure 2 as alternative paths. In such an embodiment, the system can include the bypass valve or two transfer feeders that are controlled separately after the de-aeration stage allowing the biomass to optionally proceed through solvent extraction or bypass solvent extraction and proceed directly to preheating. Such a system can be used when a part of the biomass that will be processed includes valuable extracts while another part does not include such extracts.
    One or more of the EM / EA 29 treatments (such as PEF, US, MW) can be used in connection with one or more of the washing systems 12, 14, 16 to enhance the performance of the washing systems 12, 14, 16. For For example, one or more of the solvent washing systems 12, 14 or the water washing system 16 may include a pulsed electric field generator to apply PEF to the biomass before it enters, or as it passes on, the conveyor belt solvent wash. PEF can create holes in the cell walls that can allow faster extraction of biomass materials. PEF parameters vary with the raw material, but in some embodiments they may include field strength of 10 to 20 kv / cm, pulse duration of 5 to 10 microseconds, pulse period of 10 to 20 milliseconds, and / or exposure time from 0.1 to 0.2 seconds, for example.
    Devolatilization
    Modalities of the invention include a devolatilization process. In some embodiments, volatile components (such as low molecular weight organic waste and some oils and lipids) are removed from biomass by single or multiple stage steam distillation or rapid volatilization. In some embodiments, a unique form of steam explosion using a very rapid continuous steam heating process can be used to break down biomass cells. This process subjects the biomass material to high temperature and moderate to high pressure, causing the water in the cells to expand and vaporize, leading to an increase in internal pressure sufficient to rupture or explode the cells. In other embodiments, the biomass is disrupted using a combination of steam and one or more of the EM / EA treatments in a similarly continuous process.
    The continuous flow steam blast process (or sharp steam rupture) provides several advantages, which include continuous passage of biomaterial through the system, delicate control of processing conditions, improved energy conservation, and the ability to remove and collect volatile components contained in biomass. The continuous-flow steam explosion (or sharp burst) process can be performed using superheated steam, as in a superheated steam tube like a steam loop. The biomass is fed into the steam tube in which it is exposed to superheated steam, rapidly increasing the temperature of the biomass. In addition, for cell rupture by simple steam heating, the rupture can be caused by cavitation and poration and permeabilization of the cell wall. Because of the speed of heating, the vapor is unable to diffuse out of the cell before it causes the cell to burst. Thus, while the cells are still under pressure and high temperature in the steam tube, the biomass cells burst or explode, opening the cells. By disrupting the cell structure, the components become more accessible, allowing the subsequent fractionation of hemicellulose, cellulose, and lignin.
    In some embodiments, the superheated steam is at a temperature between about 120 and about 220 degrees Celsius and a pressure between approximately 600 kPa (6 bar) and approximately 1,600 kPa (16 bar). In some embodiments, the temperature is preferably between 150 and 190 degrees Celsius and the pressure from 1,000 kPa (10 bar) to 1,500 kPa (15 bar). At this temperature and pressure, the biomass can be heated very quickly without forming an animal charcoal or undergo significant hydrolysis of the carbohydrate fractions.
    Overheated steam can be poured through a pipe, tube or similar structure. For enhanced energy efficiency, steam can flow in a continuous loop under the force of a fan or fan. When the biomass is injected into the pipe, it is carried in the steam and is conducted with the steam so that the biomass particles are suspended and move through the pipe without fixing to the bottom of the pipe. In addition, steam and biomass can be conducted through the system at a high speed, generally at speeds of 10 to 25 m / s and preferably at speeds of 15 to 20 m / s. By using this process of carrying overheated steam, the biomass heats up much faster than with a batch or stationary process, allowing for the rapid heating required for the steam explosion to occur. This can create a highly turbulent flow, which, together with the high temperature steam and high surface condensation film coefficients, allows faster transfer of heating from the steam to the biomass. It is believed that the vapor condenses on the outside of the biomass particle, causing transfer of heat to the biomass by conduction, convection and radiation.
    In addition, the use of EM / EA treatments, with high speed steam, can substantially increase the energy transfer rate, from hourly periods or tenths of minutes to batch processes in seconds, with PEF, for example, acting to open cell membranes in microseconds. EM / EA treatments can be applied to the biomass immediately before penetrating the devolatilization tube or as they pass through the devolatilization steam tube. A part of the tube can be a pulsed electric field generator, ultrasonic energy generator or microwave generator, which directs the EM / EA treatment in the tube. In some modalities, PEF can be applied to biomass during devolatilization. Again, PEF parameters vary with the raw material and can include field strength of 10 to 20 kv / cm, pulse duration of 5 to 10 microseconds, pulse period of 10 to 20 milliseconds, and / or exposure time of 0 , 1 to 0.2 seconds. In other modalities, ultrasonic energy can be applied to biomass during devolatilization. US parameters can include frequency from 20 to 40 kHz and / or exposure from 30 to 90 seconds. In still other modalities, both PEF and ultrasonic energy can be applied to biomass during devolatilization. Either PEF can be applied first, followed by US, or US can be applied first followed by PEF. US, for example, can heat the biomass cells from the inside out in seconds, while the steam transfers heat from the outside of the biomass to the inside. The US then allows for a faster and more efficient devolatilization process. In some embodiments, the entire process of devolatilizing the biomass can take approximately 1 and a half to three minutes (which includes approximately four to five seconds in an overheated steam loop).
    The use of a superheated steam tube as a steam loop for various reaction processes that include devolatilization and hydrolysis of hemicellulose, for example, allows precise control of temperature and pressure conditions as well as the time for carrying the biomass in the system. In addition, the transit time of the biomass in the system can be controlled by controlling the speed of the fan to increase or decrease the speed of the vapor in which the biomass is carried. Thus, the temperature, pressure and speed of the biomass can all be carefully and independently controlled to optimize the process. A single loop residence time can be on the order of 5 to 10 seconds.
    The continuous flow steam explosion opens the biomass cell structure to allow biomass fractionation and also releases the volatile and non-carbohydrate components of the biomass, such as acids, oils, and terpenes (for example, turpentine and essential oils). The volatile components are vaporized by the high temperature and also subjected to steam distillation due to the superheated steam. The steam distillation process reduces the effective boiling point of certain volatile components, such as organic components such as oils, at a temperature that is lower than the boiling point of pure component at atmospheric temperature, resulting in the volatilization of the components in a lower temperature than would otherwise be required. This makes it possible to remove more volatile components than would otherwise be possible by heating to a specific temperature only in the presence of overheated steam.
    Volatile components released by the water vapor explosion process can be collected, such as allowing water vapor to pass to a gas collection device such as a condenser, such as a direct contact condenser, gas scrubber or similar device. The gas collection device can be supplied in line inside the tube or water vapor cycle to allow a continuous and uninterrupted flow of biomass material and water vapor and can operate continuously, which allows water vapor and biomass flow continuously through. In addition to the removal of volatile components, any remaining oxygen or any inert gases within the biomass can be removed by the water vapor explosion process as well, thus executing or completing the de-aeration process. The process of superheated water vapor of continuous flow and, therefore, results in devolatization through distillation of water vapor in equilibrium, explosion of water vapor (with or without EM / EA treatment) from the biomass cells, and complete de-aeration of biomass.
    Examples of continuous water vapor reactors that can be used for the devolatization process include, for example, conventional multiple or single tube reactors with or without static or rotary internals, screw conveyors or extruders, fluidized bed reactors such as bubbling, jet, or circulating bed reactors, ablative reactors, and, in general, any continuous single-pass system.
    Before entry, the water vapor reactor used for the explosion of water vapor in continuous flow, the biomass is at atmospheric pressure, while inside the water vapor reactor it is at a high pressure. Therefore, the biomass needs to be injected into the water vapor reactor by using a solid feed system that can operate against this pressure differential. In one embodiment, the solids feed system is a type of lockable / discharged oil preheat tank system. This system is a batch system operated in a fast cyclical manner, but it can be made to operate in an essentially smooth continuous manner by adding a conveyor system such as a screw or rotary feeder. In another embodiment, the solids feed system is a solids pump, a centrifuge device in which friction is used to move solids in a plug flow. Such solid feed systems can be used at any of the various stages described in this where a solid feed system is required, or at any location where the biomass is transferred from one system or step to another.
    A modality of a system and process for high-pressure continuous-flow water vapor explosion (and improved cell rupture) is shown in Figure 3. The prepared biomass, such as the biomass that results from the process shown in Figure 1 or Figure 2, is fed into a solid feed system 30. The biomass is then injected into the continuous water vapor cycle 32 at a water vapor cycle inlet 34. A blower 36 in connection with the cycle water vapor 32 pushes water vapor and biomass dragged through the water vapor cycle 32. Within the water vapor cycle 32, biomass is rapidly heated by the use of superheated water vapor in high temperature and pressure, optionally together with one or more of the treatment EM / EA generators 33, to interrupt or explode a cell structure of the biomass, release the volatile components and prepare the biomass for fractionation, while the biomass is transported inside the water vapor cycle 32. The water vapor exploded, or interrupted, the biomass travels through the water vapor cycle 32 to a separator inlet 38, in line with the water vapor cycle 32 to enter in separator 40. Separator 40, like a cyclonic separator, separates solid biomass from water vapor and volatilized components. The water vapor leaves the separator 40 along with the volatilized components and inert gases through a first separator outlet42 to continue circulating through the water vapor cycle 32. The water vapor and the volatilized components pass to a gas collection device 44, such as a spray tower, which purifies the volatilized soluble components. Other remaining inert gases and vapors pass in a portion of these, along with a similar proportion of the water vapor, are removed from the pressure controlled cycle of the pressure control device 46. The pressure control device 46 can compensate for a increased cycle pressure caused by inert gases and low-melting volatile vapors by venting some of the gases, vapors (and water vapor) to balance the pressure in the cycle. Condensable components can then be condensed out using a condenser or removed by a separate gas scrubber, for example, for recovery. The remaining water vapor and gases recirculate back to the blower 36 and through the water vapor cycle 32 for reuse. The exploded biomass exits separator 40 through a second separator outlet 48 to exit water vapor cycle 32 and pass to the next stage of the fractionation process. In some modalities, biomass goes through the hemicellulose hydrolysis stage after devolatization.
    In some embodiments, the solids leaving separator 40 are fed into one or more additional water vapor explosion systems, such as one or more water vapor cycle systems 32 and separator 40, to repeat the process explosion of water vapor in any biomass that remains unexploded. In such embodiments, any additional volatile components can be collected again and the fully blown (or opened) solid biomass can then be passed on to the next stage of the fractionation process.
    Hemicellulose hydrolysis
    After the preparatory steps are complete, the biomass is now ready to be subjected to the extraction of hemicellulose. Hemicellulose can be removed from biomass by any method or combination of methods, such as hot water, acid or alkali processes. In some modalities, hemicellulose is removed by hydrolysis using superheated water vapor. In some modalities, the entire preparatory steps may take approximately seven minutes to nine and a half minutes with oil extraction or four and a half to seven minutes without oil extraction.
    In some modalities, hemicellulose is hydrolyzed by the use of superheated water vapor, in a continuous process, such as by carrying the biomass in a continuous water vapor reactor (for example, a cycle, a tube, etc.). ). Examples of continuous water vapor reactors that can be used for hemicellulose hydrolysis include, for example, conventional multiple or single tube reactors with or without static or rotary internals, screw conveyors or extruders, fluidized bed reactors such as bubbling, jet, or circulating bed reactors, ablative reactors, and, in general, any continuous single-pass system.
    In some embodiments, water vapor is applied to the biomass at a pressure of about 1000 to 3500 kPas and a temperature of about 170 to 250 degrees Celsius. In other modalities, the pressure is 2300 to 3200 kPas and the temperature is 220 to 240 degrees Celsius. Temperature and pressure are sufficient to hydrolyze hemicellulose while minimizing or preventing degradation of the biomass material. While the reaction kinetics of both hydrolysis and degradation are functions of time, temperature and conditions such as pH, these can exhibit different optimums, so that it is possible to maximize the recovery of the product's sugars by selecting operating conditions. appropriate. In some modalities, a single water vapor reactor is used, while in other modalities, two or more vapor reactors are used in series with the conditions of each selected reactor to obtain different products.
    In some embodiments, the hydrolysis step employs one or more of the EM / EA treatments, as discussed elsewhere in this document, to improve heat transfer and assist in the decomposition of hemicellulose. For example, one or more PEF, US or microwave can be applied to the biomass during, or before, the hemicellulose hydrolysis reactor. In some embodiments, ultrasonic energy is produced by an ultrasound generator inside, or immediately before, the reactor to direct ultrasonic energy into biomass as it enters, or passes through, the reactor. Ultrasonic energy parameters vary with raw material and the desired reaction or products and can typically be: frequency from 20 to 40 kHz or from 200 kHz to 1 MHz; duration of 1 to 5 seconds or from 3 to 90 seconds, ultrasonic energy (or microwave) can provide a method of supplementary heating to biomass in the
    hemicellulose through O heating of biomass internally, making The reaction in hydrolysis in faster hemicellulose.In some modalities, The hydrolysis in
    hemicellulose begins at a first stage or location of superheated water vapor, such as a continuous water vapor tube or cycle, and then continues at a second location or stage of saturated or overheated water vapor, such as the outer side tube or water vapor cycle. In some embodiments, this second stage is at approximately the same temperature and pressure as the first stage, with the second stage acting as a retention system, which allows the hemicellulose reaction that started in the reaction chamber or water vapor cycle to achieve perfection. The biomass can be kept in this retention system long enough for the hemicellulose hydrolysis reaction to reach perfection, such as about one to two minutes, for example, at a desired temperature. The completion of the hydrolysis reactions can be performed at a lower temperature, however longer residence times would be required to complete the hydrolysis. The holding system can comprise a holding tank, for example, or it can be a conveyor belt system, such as a slow moving belt system. Alternatively, the complete hemicellulose hydrolysis process can occur within a single stage or location, such as by maintaining the biomass in a reaction chamber or to keep it inside the tube or water vapor cycle for a longer time , enough for the hemicellulose hydrolysis reaction to reach perfection. However, the length of the water vapor / pipe cycle is directly proportional to the cost of the system, so it may be more expensive to extend the pipe or water vapor cycle than to include a separate second stage on the outside of the water cycle. water vapor / tube.
    The reaction process begins in the superheated water vapor environment. However, the two stages of the reaction do not necessarily correlate with the two stages of the superheated water vapor process described above. The superheated cycle / tube section is used to provide heat transfer to initiate the reaction, aided, where desirable, by EM / EA treatments. Therefore, the reaction parameters can be determined based on economy and convenience. It should be worth noting that hemicelluloses and celluloses are not the only, pure molecules, but mixtures of polymers, copolymers and cross-linked polymers, formed from numerous monomer sugars. Each of these polymers has its own hydrolysis kinetics.
    In some embodiments, two or more continuous superheated hemicellulose vapors are supplied in series. The first reactor may be at a lower temperature than the second reactor. If a third reactor is used, then the temperature of the second reactor may be lower than that of the third reactor. For example, the first hemicellulose reactor can partially hydrolyze hemicellulose (by using a lower temperature and / or a shorter reaction time than the second reactor), which produces oligomers, such as oligomers that have 2 to 20 sugars. Those oligomers and other products would then be removed, such as by leaching or a high pressure press, and the remaining solid component would then proceed for further processing. In the second hemicellulose reactor, hemicellulose hydrolysis can be completed, which thus produces hemicellulose sugar monomers.
    The hydrolyzed hemicellulose is then removed from the biomass. C5 and some C6 sugars produced by hemicellulose hydrolysis are generally water-soluble and can be dissolved in the surrounding water and absorbed into the biomass after exposure to superheated water vapor. This solution can be a relatively complex sugar solution, which comprises the particular monomer sugars of the selected raw material, plus some hemicellulose oligomers and some sugars, oligomers, etc. celluloses and sugar derivatives (anhydrous sugar, etc.). Additional contaminants can include residual volatiles, such as acetic acid, alcohols, etc. and any other soluble component such as amino acids, mineral salts, etc.
    In some embodiments, sugars are removed from biomass in a single stage in multiples, by using water and additional washing sequences and separating liquid and solid. For example, C5 and C6 sugars can be removed by using a flow of water against the current to leach the C5 and C6 hemicellulose sugars from biomass solids. In some embodiments, the C5 and C6 sugars can be removed after the first pressure drop, such as between about atmospheric and about 200 kPas, and then vent the vapors to balance a quantity of the water containing the dissolved sugars. The balanced water vapor, which will contain carried sugar-laden liquor, can be condensed in a direct or indirect condenser and the recovered liquor sent to the sugar recovery. The hydrolyzed hemicellulose sugars are then leached from the biomass. In some embodiments, low pressure leaching employs a flow of water against a current to remove dissolved hemicellulosic sugars. In other embodiments, the dissolved hemicellulosic sugars can be removed by using one or more high pressure washing and separation stages, such as by using extrusion or compression equipment such as high pressure screw presses, and washing equipment. such as screws or counter flow conveyors. In some embodiments, dissolved hemicellulosic sugars can be removed by using both press and low pressure leaching processes. In some embodiments, the entire process of hemicellulose hydrolysis and removal can take approximately one and a half to three minutes.
    The step of leaching or expressing the biomass for the removal of the hemicellulosic sugars and the separation of the biomass into a liquid component and a solid component can be carried out by means of concurrent current or counter current extraction equipment, such as a conveyor belt extruder single or double screw, a vertical plate extractor, a rotary extractor, or a centrifuge extractor, for example.
    Isolated hemicellulose sugars including C5 and C6 sugar monomers and oligomers (and derivatives such as anhydrous sugars, aldehydes, etc.) are useful as individual products and have several commercial uses. In some embodiments, some C5 sugars and sugar derivatives can be used for fermentation, such as for the production of alcohols, including ethanol and high alcohols, such as butanol. Such fermentation processes can be carried out in conjunction with the fractionation process or can be carried out separately. In some embodiments, the isolated C5 sugars can be further processed, such as for conversion to other chemicals. For example, C5 sugars can be converted to furfural. The hemicellulose hydrolysis products can also be passed for further processing in parallel with, or in conjunction with, cellulose hydrolysis products. Some of these processes are identified later, in the discussion of cellulose processing.
    A modality of a two-stage system and the process for hydrolysis of water vapor from hemicellulose of continuous flow is shown in Figure 4. Biomass, like the devolatized biomass produced by the system in Figure 2, passes to a feeding system of solids 50, as the solid feed systems described previously. The solids feed system 50 injects biomass into the continuous water vapor cycle 52 at the water vapor cycle entrance 54. Water vapor and entrained biomass are moved through the water vapor cycle 52 through the blower 56, which circulates the water vapor through the water vapor cycle 52. The biomass flows in a turbulent way and heats rapidly within the water vapor cycle 52, beginning the hydrolysis of hemicellulose. Again, an EM / EA 58 treatment generator can also be optionally employed in this cycle. The biomass passes through the water vapor cycle 52 through the separator inlet 60 to the separator 62, such as a cyclonic separator, which separates the water vapor from the biomass. Water vapor exits separator 62 through a first separator outlet 64 to continue circulating through water vapor cycle 52. The heated biomass exits separator 62 through a second separator outlet 66 and passes into the system retainer 68, which in the modality shown is a slow moving screw conveyor at the same temperature and pressure as the water vapor cycle 52. Hemicellulose hydrolysis continues to completion within the retention system 68. At the end of the retention system 68, the biomass is moved to a solids feeding system 70 and in the hemicellulose sugar delivery system 72. In the embodiment shown, water flows through the biomass to wash the sugars in a counter-current manner as the biomass moves along the conveyor belt. The water leaves the leaching system for the recovery of hemicellulose sugars. This low pressure leaching can take approximately four and a half to five and a half minutes. Thus, hemicellulose sugars can be separated from water by conventional distillation or by techniques such as pervaporation and filtration (using membranes), reactive distillation or extraction, for example. The solid biomass from which the hemicellulose was removed and which now includes cellulose and lignin passes out of the leach system 72 and continues for further processing. The solid biomass can include very little hemicellulose, such as 5% to 10% by weight of hemicellulose. In some embodiments, the solid biomass is used to remove cellulose sugars, as in the system shown in Figure 8.
    An alternative modality is shown in Figure 5. As in Figure 4, hemicellulose hydrolysis is performed using a water vapor cycle and a screw conveyor. In this alternative embodiment, the biomass containing the hemicellulose sugars passes from the retention system 68 to a first high pressure screw press 74 to remove water from the biomass, and then to mix and wash the screw 76. A second screw press high pressure 78 is shown in Figure 8, where it also functions as a feed screw 81 for the drying stage. This high pressure expression can take approximately one and a half to three minutes.
    An alternative system for hemicellulose hydrolysis is shown in Figure 6 which has two hemicellulose reactors in series for stage one. The first hemicellulose reactor and hemicellulose sugar leaching system are as described with reference to Figure 4, although the reaction conditions (such as temperature, pressure and reaction time) can be modified so that the hemicellulose hydrolysis is incomplete. The hydrolyzed hemicellulose products of the first hemicellulose reactor are leached by the leach system 72 and the residual solids including the hydrolyzed hemicellulose, cellulose and lignin are passed to the second hemicellulose hydrolysis reactor. The residual solid is pressurized again by using a solid feed system such as a lockable / discharged oil preheat tank system. The second hemicellulose reactor includes the same components as the first hemicellulose reactor but can apply different reaction conditions. For example, the time, temperature, or pressure can be such that the hydrolysis of hemicellulose is complete. The hemicellulosic sugar product can be monomeric sugars, for example, and the residual solid can be cellulose and lignin with only a small component of hemicellulose, such as less than 10%. In the modality shown, the second hemicellulose reactor includes a second solid feed system 250, a second cycle of continuous water vapor 252 that has an inlet 254 for the insertion of biomass and a blower 256 for circulating the water vapor . EM / EA treatments can be applied by an EM / EA 258 treatment generator. A second separator 262 includes an inlet 260, a first separator outlet 264 to cause water vapor to escape and a second separator outlet. 266 to pass the biomass to a second retention system 268 and then to a second solid feed system 270 and a second hemicellulose sugar delivery system 272.
    An additional alternative modality is shown in Figure 7. In this modality, as in Figure 6, there are two hemicellulose reactor loops in series. In this modality, however, after leaving the retention system 68, the water including the hydrolyzed hemicellulose is removed by using high pressure screw presses as in Figure 5. A first high pressure screw press 74 removes water from the biomass, followed by a mixing and washing screw 76. A second high pressure screw press 7 8 is shown after the first hemicellulose reactor, while the second high pressure screw press 78 followed by the second hemicellulose reactor can be seen on Figure 8, where it also functions as a feed screw 81 for the drying stage. As in Figure 6, the biomass is pressurized again before entering the second hemicellulose hydrolysis reactor by the high pressure screw press 78.
    In some embodiments, the solid component remaining after removal of hemicellulosic sugars is further processed to remove cellulosic sugars, as per the processes described herein. In other embodiments, the solid component including cellulose and lignin and relatively free of hemicellulose, such as having less than 10% hemicellulose, can be used for other processes such as fiber board production. The cellulose and lignin solid can be combined with a traditional resin such as urea or formaldehyde. Alternatively, the hemicellulose obtained as described herein can be converted to a resin by separate chemical processing and combined with the cellulose and lignin solid to produce the fiber board.
    Cellulose hydrolysis
    In the modalities in which biofaction is continuous, cellulose and lignin in the remaining solid are separated from each other below. This can be done by solubilizing lignin, using enzymatic or acidic hydrolytic processes (diluted or concentrated) or by high temperature pyrolytic processes. In some embodiments, cellulose biomass is subjected to instant thermolysis in order to want the bonds of cellulose and lignin, and simultaneously hydrolyzes the cellulose and vaporizes the hydrolysis products.
    After removing the hemicellulose, as in the process shown in Figures 3 to 7, the remaining solid biomass includes primarily cellulose and lignin. In many embodiments, on a dry basis, the remaining solid biomass is about 60 to 70% lignin and 30 to 40% cellulose, with small amounts of insolubles, such as inorganic salts. In some embodiments, solid biomass has its water removed to remove loose water on the surface, as may be required for further processing. For example, water can be removed using a high pressure press. In some embodiments, solid biomass has a water content of more than about 60%, such as about 60 to 75% prior to removal of water. After removing water, the water content of the biomass can be reduced
    to less than about 60%, such as about 50 to 60%. In some modalities, O solid with Water removed can so be dry by use in a reactor steam overheated water (for example, one cycle, one pipe,
    etc.). The water removal process produces high pressure water vapor. This additional water vapor can be recovered to be used as energy, and the pressure used in the water removal process can be determined based on the energy recovery requirements. This energy recovery can occur through the direct use of water vapor in another part of the fractionation process. Additionally or alternatively, energy can be recovered after transferring heat to a clean fluid, such as through a pressure reducing turbo-generator to generate power. Systems that can be used for the drying step of the solid biomass component include continuous water vapor reactors such as conventional single or multiple tube reactors with or without static or rotary internals, screw conveyors or extruders, bed reactors fluidized such as bubbling, jet, or circulating bed reactors, ablative reactors, and, in general, any continuous single-pass system.
    The use of a water vapor tube or cycle for drying also allows the drying process to be continuous. Alternatively or additionally, in some modalities, drying can be carried out by direct contact with a stream of dry and hot gas (such as flue exhaust gases) or by a range of indirect continuous drying systems, including belt and rotary dryers. The biomass can be dried to a water content of about 1 to 10%, and like a water content of about 2 to 4%. In some embodiments, the drying process can take one to two minutes (including four to five seconds in the water vapor / tube cycle).
    In some embodiments, the remaining solid biomass is further processed to reduce its size. For example, biomass can be cut into small pieces using an attractor or grinder to reduce the solid to a fine powder. In some embodiments, a size range of about 0.5 to 5 mm in diameter can be used while in other embodiments, a size range of about 2 to 3 mm in diameter can be used. The size reduction is used for the purpose of ensuring that the particularly quickly reaches the temperature at which thermolysis occurs, such as within about 0.5 to 3 seconds. The friction of the biomass can be used in the modalities in which the biomass will be subjected to instant thermolysis, for example. In the modalities in which cellulose thermolysis includes EM / EA treatments, drying and / or friction of the biomass may be optional.
    Instantaneous thermolysis can then be performed by subjecting the biomass to a very high superheated water vapor or inert gas, or a combination of water vapor and inert gas, optionally together with one or more of the EM / EA treatments. EM / EA treatments can be used to increase the heat transfer rate and to assist in breaking the microcrystalline structures of the most complex and largest polymer molecules. In some embodiments, one or more PEF, ultrasonic energy or microwave energy can be applied to the biomass immediately before it enters or as it passes through the cellulose reactor or any subsequent reactors. As such, a portion of the reactor may include an EM / EA treatment generator to direct the EM / EA treatment to the biomass before or as it passes through the reactor tube, for example. In some modalities, microwave energy is applied, while in other modalities ultrasonic energy is applied, within yet other modalities both microwaves and ultrasonic energy are applied to biomass in, or before, the same reactor. Microwaves and ultrasound energy can be applied in any order, separately, in proximity, consecutively or simultaneously. This combination of treatments can be particularly useful, as ultrasound energy can break cellulose crystals, while microwave energy can provide rapid heating. In some embodiments, ultrasound energy can be applied at a frequency of 20 to 40 kHz or 200 kHz to 1 MHz and the duration from 1 to 5 seconds or 30 to 90 seconds. Microwave energy can be applied at a frequency of 0.8 to 3 GHz and lasts from 1 to 10 seconds. In some embodiments, when EM / EA treatments are used in the cellulose hydrolysis step, the steps of drying and / or rubbing the biomass before feeding it into the cellulose reactor can be omitted.
    Instantaneous thermolysis can be performed using a continuous process, such as feeding the biomass into a continuous water vapor reactor. In some embodiments, the reactor includes only water vapor as the gas carrier. In other modalities, water vapor is used in combination with an inert gas to hydrolyze and carry the biomass. Examples of inert gases that can be used include CO2, CO, nitrogen, hydrogen, or combinations thereof. Certain carrier gases can result in reactions that favor the production of certain cellulose products. As such, the gas carrier or gases can be selected and used according to the desired products. For example, the use of hydrogen as a gas carrier can result in the production of less oxygenated bio oils.
    In some embodiments, superheated water vapor and / or gas can be applied to the biomass at a temperature between about 350 and about 550 degrees
    Celsius. In some embodiments, superheated water vapor and / or gas can be applied to the biomass at a temperature between about 400 and about 450 degrees Celsius. Actual temperatures are dependent on the raw material and the desired products. In some embodiments, superheated water vapor and / or gas can be applied to the biomass at a pressure of between about 0 kPas and about 400 kPas, as can the pressure between about 100 kPas and about 200 kPas, depending on pressure losses in the system. By using the appropriate temperature and residence time, the bond between lignin and cellulose is broken and the cellulose is hydrolyzed by water vapor in C6 sugars and other volatile compounds that are vaporized. The solid that remains after vaporizing the cellulose consists of a lignin charcoal. In some embodiments, the presence of water vapor and the use of a temperature that is low enough can be selected to substantially prevent pyrolysis of the biomass, which would cause cellulose to form a much higher proportion of various hydrocarbons such as piches, oils and gases. Therefore, in such embodiments, the temperature of the thermolysis reaction may be high enough for hydrolysis but not so high or the cellulose will otherwise pyrolyze and the chemical composition of the products will be greatly altered. In some embodiments, thermolysis can take approximately 30 seconds to one minute (including one and a half to five seconds in the reactor).
    In other modalities, cellulose thermolysis can be performed using two or more continuous superheated water vapor and / or gas reactors. The reaction conditions of the first cellulose reactor, including temperature, pressure, reaction time, and gas carrier, can be selected so that the cellulose hydrolysis reaction favors the production of one or more first cellulosic products. For example, The first cellulose reactor can produce cellulose oligomers or a higher proportion of a specific C-6 sugar. The second cellulose reactor and any subsequent cellulose reactors can have different reaction conditions, such as to complete the cellulose hydrolysis. In such embodiments, the second reactor can be considered a second cellulose reactor hydrolysis. For example, the first cellulose reactor can be at a temperature of 350 to 500 ° C while the second cellulose reactor can be at a temperature of 450 to 550 ° C, with the temperature in the first reactor being less than in the second reactor. In other embodiments, the second reactor may provide conditions for pyrolyzing lignin, in which case the second reactor may comprise a lignin pyrolysis reactor. This can follow complete cellulose hydrolysis. For example, the first reactor can hydrolyze cellulose at a temperature of about 350 to 550 ° C and the second reactor can pyrolyze the lignin at a temperature of 450 to 650 ° C, with the temperature of the first reactor lower than that of the second reactor. In yet another embodiment, the cellulose hydrolysis can be performed partially from a first cellulose reactor hydrolysis to produce a first cellulosic sugar product and then the cellulose hydrolysis can be completed by a second cellulose reactor hydrolysis. A third reactor (a lignin pyrolysis reactor) can then pyrolyze the lignin. In such embodiments, the first reactor can be at a temperature of 350 to 500 ° C, the second reactor can be at a temperature of 400 to 550 ° C, and the third reactor can be at a temperature of about 450 to 650 ° C, with the temperature in the first reactor lower than the second reactor and the temperature in the second reactor lower than that of the third reactor.
    In some embodiments, the final reactor can treat the remaining lignin fraction after cellulose removal by one or more cellulose reactors to gasify the lignin. Such a reactor can be a continuous water vapor reactor like those used for cellulose thermolysis, but it can apply the highest temperature such as about 900 to 1200 ° C to produce hydrogen and carbon monoxide that can be used for chemical conversion processes.
    The vaporized and volatile C6 sugars can be separated from the remaining biomass and collected. In some embodiments, the remaining biomass (such as lignin charcoal) and vapors are passed inside a separator to separate vapors from solids, such as a cyclonic separator, which can be in line within the vapor cycle / tube. Water. The separate steam includes the hydrolyzed cellulosic vapors, which can then be condensed, such as by a direct contact condenser, purifier, or similar apparatus. These vapors also contain significant thermal energy, which can be recovered. Cellulosic sugars can then be extracted from the condensed liquid, as with any of the technologies listed above for hemicellulose products. Separated cellulosic sugars can include glucose, levoglucosan, and levulinic acid, for example. Cellulosic sugars and other products collected can then be used for a variety of commercial purposes or for further processing, such as fermentation to produce alcohols, in conjunction with the fractionation process or separately. Other downstream technologies that can use the primary products of this fractionation process include Virent's Water Phase Reform Process (for synthetic gasoline, jet fuel and diesel); Segetis Binary Monomer Technologies; and other catalytic conversion processes and chemical or biochemical reaction processes.
    The solid that remains after cellulose hydrolysis is a lignin charcoal. Lignin coal can be further processed. For example, lignin can be chemically converted into other products, such as phenols, soluble lignosulfates and, more generally, in the range of aliphatic, cyclic and aromatic raw materials. Alternatively, some types of lignin can be pyrolyzed to produce phenols for synthetic resins. In some embodiments, lignin can be fed into a reactor such as the cellulose reactor, as a final reactor. This lignin reactor can be used to pyrolyze lignin to produce phenolic products, for example. In other embodiments, lignin can be burned to produce energy, such as for the operation of the fractionation system. In still other modalities, lignin can be gasified to produce hydrogen and synthesis gas, with hydrogen found in its use in reducing reactions of some of the other primary products.
    Thermolysis and pyrolysis can be carried out in single trapped flow tube reactors or fluidized bed reactors. Examples of fluidized bed reactor which can be used include bubbling fluidized bed or circulating fluidized bed, or in special reactors, such as a rotary cone reactor or other ablative type reactor. In embodiments that include a lignin gasification reactor, the reactor can be any of the above reactors used for thermolysis or pyrolysis, or it can be a co-current or counter-current fixed bed reactor, for example.
    Fluidized bed reactors generally require an inert medium and heat the biomass through contact with a preheated particulate medium. The inert medium may also have some catalytic activity. The biomass is introduced into the inert bed, which is fluidized by a stream of hot gas that passes through it.
    A modality of a system and process for hydrolysis and cellulose fractionation is shown in Figure 8. The following hemicellulose hydrolysis, as with the system shown in Figures 3 to 7, biomass can be prepared by rapid thermolysis when drying the biomass. The biomass is passed through the final dehydration high pressure rocker 78 which also functions as a lead screw, for example, and inside a superheated water vapor cycle 80 through a steam cycle input. water 82 for superheated water vapor to dry the biomass. The superheated water vapor cycle 80 includes a blower 84 which causes water vapor and trapped biomass to circulate through water vapor cycle 80 to separator 86, such as a cyclonic separator, which separates water vapor from biomass. The separator includes an inlet 88, a first outlet 90 through which the water vapor exits to recirculate in the water vapor cycle 80, and a second outlet 92 through which the dry biomass exits. After leaving the separator, the biomass can pass through the shredding system 94. From the shredding system 94, the biomass passes inside a solid feed system 96, like those described above, and then inside the steam reactor. of water 100 through the entrance of water vapor reactor 102 for the separation of cellulose from lignin, the hydrolysis of cellulose in vapors of C6 and other volatile sugars, and the formation of lignin coal within the steam reactor d ' water 100. The thermolysis reactor can also optionally contain one or more of the treatment generator EM / EA 103. The vapors of cellulose and lignin coal pass through the water reactor 100 to a separator 104, such as a cyclonic separator, in which C6 sugar and other volatile vapors are separated from lignin carbon. The separator includes an inlet 106, a first outlet 108 through which the vapor of separated C6 sugars and water vapor leave the separator, and a second outlet 110 through which the lignin coal exits the separator.
    An alternative embodiment is shown in Figure 9. As in Figure 8, the biomass first passes through a superheated water vapor cycle 80 to dry and a shredding system 94. The solid material including cellulose and lignin then passes inside of a first water vapor reactor 100 for cellulose hydrolysis and then passes through the separator inside a second water vapor reactor 200. The conditions of the first water vapor reactor 100 can only partially hydrolyze cellulose , in which case the first steam reactor 100 is a first cellulose hydrolysis reactor and the second steam reactor 200 can be a second cellulose hydrolysis reactor that completes cellulose hydrolysis. Alternatively, the first steam reactor 100 can complete the cellulose hydrolysis so that the remaining solid is comprised of only lignin, in which case the second steam reactor 200 can be a lignin reactor for pyrolysis of lignin. The product resulting from the second reactor can be separated by a separator 110, in phenols and coal.
    In Figure 9, the second water vapor reactor 200 is an overheated tube of water vapor like the first water vapor reactor 100. The remaining biomass passes through the first separator 104 and inside the second steam reactor d 'water 200. The second steam reactor 200 includes an inlet 202 and an outlet 206 through which the remaining biomass passes to a second separator 204. The second separator includes a first outlet 208 and a second outlet 210. In the modality shown, the first water vapor reactor 100 completely hydrolyzes cellulose and the second water vapor reactor 200 pyrolysis lignin to produce phenols. The phenols leave the separator as steam through the first outlet 208 while the remaining lignin coal exits the separator through the second outlet 210. In alternative modalities, or under alternative conditions, the first water vapor reactor 100 can incompletely hydrolyze the cellulose and the second water vapor reactor can complete the cellulose hydrolysis with the cellulosic products leaving the second separator 204 as steam through the first outlet 208 and the lignin coal that exits through the second outlet second outlet 210.
    In some embodiments, biofaction may include a branch after removal of hemicellulosic sugars and before the remaining cellulose and lignin solid proceeds to cellulose thermolysis. In this field, a side stream of cellulose and lignin solid can be diverted for separate processing. For example, the side stream can subject the solid to chemical treatment to separate cellulose and lignin. For example, a standard wood pulp treatment, such as the sulfite process (using sulfurous acid salts such as sulfites or bisulfites) or the Kraft process (using sodium hydroxide and sodium sulfate) or the National Renewable Energy Laboratory (NREL) Clean Fractionation Process (using methylisobutylketone) can be used to dissolve lignin. The resulting cellulose pulp can then be obtained as a product which can be used to produce paper or chemicals and cellulosic fibers. Such an optional side chain provides additional flexibility to the system.
    The various systems and processes shown in Figures 1 to 9 can be used individually, in combination with several other fractionation systems, or can be used together in different combinations. When used together, the systems and processes in Figures 1 to 9 can be used to form a continuous flow fractionation system for the separation of non-carbohydrates (lipids, proteins, etc.), hemicellulose, cellulose and lignin from a material of lignocellulosic biomass in which the biomass flows continuously through an entire system. The continuous system separates the lignocellulosic material into four or more separate fractions, isolating non-carbohydrates, hemicellulose sugars, cellulose and lignin sugars individually.
    A flowchart showing an example of how the process can be used to completely fractionate lignocellulosic biomass is depicted in Figure 10. A single system can be used by which the various options can be included and by which they can be circumvented as desired. In this way, the system provides a high degree of flexibility, capable of accommodating any raw material and adjusted to produce desired fractionation products. As shown in the example in Figure 10, the first step is the preparation of biomass 302. This step may or may not be necessary, depending on the nature and source of the biomass. If extractives are desired, the next step is to remove extracts 304. If no extractives are desired, this step can be omitted or bypassed. The biomass then moves on to the next step, which is 306 devolatilization. The volatiles released during this step can be isolated in the 308 volatile isolation step. The biomass then proceeds to the hemicellulose hydrolysis steps 310 and liquid and component separation solid 312. The liquid component can then proceed to the hemicellulose product isolation step 314. If hemicellulose hydrolysis is not completed, the solid can then proceed through the hemicellulose hydrolysis steps 310 and separation of the liquid and solid components 312 again, however, this will occur in a second hemicellulose reactor and can use different reaction conditions, such as increased temperature and / or time. When hemicellulose hydrolysis is complete, the solid biomass moves to cellulose hydrolysis step 316. Vapors produced by cellulose hydrolysis are isolated in the cellulosic product isolation step 318. If cellulose hydrolysis is incomplete, biomass The remainder can repeat the cellulose hydrolysis step, however the process will take place in a second cellulose hydrolysis reactor and can use different reaction conditions, such as increased temperature and / or time. If cellulose hydrolysis is complete, the resulting lignin coal 320 can be obtained as a final product, or this can proceed to the step of lignin pyrolysis 322 or gasification of lignin 324. In an alternative embodiment, after the completion of hydrolysis hemicellulose 310, the solid component can be used to produce fiber board 330.
    Heat can be supplied to the various reactors using a variety of media. For example, hot oil can be used as in conventional heating systems, with reactors that have hot oil liners. In some embodiments, induction can be used to heat water vapor and / or heat biomass. In other embodiments, infrared energy can be used for heating.
    Several approximate residence times have been provided in the present invention. In some modalities, the entire preheated biomass fractionation process is between four and a half minutes and eleven and a half minutes. In modalities that employ a low pressure process to separate hydrolyzed hemicellulose from lignin cellulose solid in the hydrolysis stage, the preheated biomass can be fractionated in approximately seven and a half minutes to eleven and a half minutes, and crude biomass can be completely pre-treated (which includes oil extraction) and fractionated in approximately fourteen and a half minutes to twenty-one minutes. In modalities that employ a high pressure process to separate hydrolyzed hemicellulose from lignin cellulose solid in the hydrolysis stage, the preheated biomass can be fractionated into approximately four-and-a-half for nine minutes, and crude biomass can be completely pre-treated (which includes oil extraction) and fractionated in approximately eleven and a half minutes to eighteen and a half minutes.
    In the foregoing detailed description, the invention has been described with reference to specific embodiments. However, it can be appreciated that several modifications and changes can be made without departing from the scope of the invention.
    Therefore, some of the features of preferred embodiments described in the present invention are not necessarily included in preferred embodiments of the invention which are intended for alternative uses.
    权利要求:
    Claims (14)
    [1]
    1. Lignocellulosic biomass material fractionation method, characterized by the fact that it comprises:
    feed the biomass continuously to a devolatilization reactor to remove volatile non-lignocellulosic components from the biomass using a superheated steam reactor at a temperature between 120 ° C and 220 ° C and a pressure between 600 and 1600 KPa (6 and 16 bar);
    after devolatilization, continuously feed the biomass prepared to a hemicellulose hydrolysis reactor to separate and hydrolyze the hemicellulose;
    continuously separating the biomass into a first solid component and a liquid component, where the liquid component includes hemicellulose hydrolyzed in water or solvent, and where the solid component includes cellulose and lignin and has less than 10% hemicellulose;
    feeding the solid component continuously to a cellulose hydrolysis reactor comprising a continuous superheated steam reactor to hydrolyze and vaporize the cellulose component; and continuously condensing the vaporized and hydrolyzed cellulose.
    [2]
    2. Method according to claim 1, characterized in that the cellulose hydrolysis reactor applies superheated steam to the biomass and a temperature of at least 300 ° C, preferably at a temperature between 350 ° C and 550 ° C.
    [3]
    3. Method, according to claim 1 or 2, characterized by the fact that the cellulose hydrolysis reactor applies pressure to the biomass from 100 to 300 kPa (1 to 3 bars).
    Petition 870190105009, of 10/17/2019, p. 7/9
    2/3
    [4]
    4. Method according to claim 1, characterized in that the cellulose hydrolysis reactor applies a mixture of steam and a gas to the solid component, the gas preferably comprising nitrogen, hydrogen, carbon dioxide, or carbon monoxide combinations thereof.
    [5]
    5. Method according to claim 1, characterized by the fact that it additionally comprises applying electromagnetic or electroacoustic treatment (EM / EA) to the solid component immediately before it enters the cellulose hydrolysis reactor and / or when it passes through of the cellulose hydrolysis reactor, the EM / EA treatment preferably including Pulsed Electric Field, ultrasonic energy, microwave energy, and combinations thereof.
    [6]
    6. Method according to claim 1, characterized by the fact that the devolatilization reactor comprises a continuous steam reactor.
    [7]
    7. Method according to claim 1, characterized in that it additionally comprises feeding the solid component to a dryer that comprises a continuous superheated steam reactor after separating the biomass in the hemicellulose hydrolysis reactor to reduce the content of water from the solid component before feeding the solid component to the cellulose hydrolysis reactor.
    [8]
    8. Method according to claim 1, characterized by the fact that it additionally comprises putting the solid component in friction after separating the biomass in the hemicellulose hydrolysis reactor and before feeding the solid component to the cellulose hydrolysis reactor.
    Petition 870190105009, of 10/17/2019, p. 8/9
    3/3
    [9]
    9. Method according to claim 1, characterized by the fact that the hemicellulose hydrolysis reactor comprises a continuous superheated steam reactor.
    [10]
    10. Method according to claim 1, characterized by the fact that the cellulose hydrolysis reactor produces a vapor of hydrolyzed cellulose and lignin coal.
    [11]
    11. Method according to claim 1, characterized by the fact that the cellulose hydrolysis reactor hydrolyzes cellulose and produces cellulosic sugar vapor and a second solid component.
    [12]
    12. Method according to claim 11, characterized in that it additionally comprises feeding the second solid component to a second cellulose hydrolysis reactor comprising a continuous superheated steam reactor.
    [13]
    13. Method according to claim 12, characterized in that the first cellulose reactor partially hydrolyzes cellulose and the second cellulose hydrolysis reactor completes cellulose hydrolysis and separates the vaporized cellulose from lignin.
    [14]
    Method according to claim 11, characterized in that it additionally comprises feeding the second solid component to an overheated steam reactor to reduce the lignin to a condensable vapor.
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    同族专利:
    公开号 | 公开日
    EP2483331A2|2012-08-08|
    US20140123973A1|2014-05-08|
    US8657960B2|2014-02-25|
    CA2775656A1|2011-04-07|
    EP2483331B1|2017-05-03|
    US9994924B2|2018-06-12|
    WO2011039635A3|2011-11-10|
    CA2775656C|2018-03-27|
    US20110100359A1|2011-05-05|
    LT2483331T|2017-07-25|
    AP2012006223A0|2012-04-30|
    BR112012007026A2|2017-03-01|
    ES2630053T3|2017-08-17|
    US9200336B2|2015-12-01|
    PL2483331T3|2017-10-31|
    AP3563A|2016-01-27|
    WO2011039635A2|2011-04-07|
    US20160068920A1|2016-03-10|
    DK2483331T3|2017-08-28|
    ZA201202754B|2013-06-26|
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    法律状态:
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2019-02-26| B06T| Formal requirements before examination|
    2019-07-23| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|
    2019-12-03| B09A| Decision: intention to grant|
    2020-01-07| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 29/09/2010, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    US24672109P| true| 2009-09-29|2009-09-29|
    US61/246,721|2009-09-29|
    PCT/IB2010/002591|WO2011039635A2|2009-09-29|2010-09-29|Method and system for fractionation of lignocellulosic biomass|
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