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    • 专利摘要:
    The invention relates to a continuous process for treating a lignocellulosic biomass before enzymatic hydrolysis, which process comprises a transfer of crushed biomass then pressed in an impregnation step with an acidic liquor, the impregnated biomass dripping over the zone containing the impregnating liquor, then the resulting wet biomass is pressed and sent to a steam explosion stage. The impregnating liquor is prepared in a dedicated zone from spent liquor resulting from the dewatering and / or that resulting from pressing before explosion. The invention also relates to the installation for implementing the method.
    公开号:FR3053969A1
    申请号:FR1656829
    申请日:2016-07-18
    公开日:2018-01-19
    发明作者:Damien Hudebine；Romain Rousset；Olivier Carnnot
    申请人:IFP Energies Nouvelles IFPEN；Institut National de la Recherche Agronomique INRA；Agro Industrie Recherches et Developpements ARD；
    IPC主号:
    专利说明:

    Holder (s): IFP ENERGIES NOUVELLES Public establishment, NATIONAL INSTITUTE OF AGRONOMIC RESEARCH Public establishment, AGRO INDUSTRIES RESEARCH AND DEVELOPMENT Limited company.
    Extension request (s)
    Agent (s): IFP ENERGIES NOUVELLES.
    FR 3 053 969 - A1 (54) PROCESS FOR TREATING LIGNO-CELLULOSIC BIOMASS BY IMPREGNATION AND EXPLOSION BY STEAM.
    The invention relates to a continuous process for the treatment of lignocellulosic biomass before enzymatic hydrolysis, process comprising a transfer of crushed and then pressed biomass in an impregnation step with an acidic liquor, the impregnated biomass dripping off. above the area containing the impregnation liquor, then the resulting wet biomass is pressed and sent in a steam explosion step. The impregnation liquor is prepared in a dedicated zone from the spent liquor from draining and / or from the pressing before explosion.
    The invention also relates to the installation for implementing the method.

    Field of the invention
    The invention relates to a process for treating lignocellulosic biomass to produce so-called second generation (2G) sweet juices. These sugary juices can be used to produce other products biochemically (e.g. alcohols such as ethanol, butanol or other molecules, for example solvents such as acetone etc ...). This process consists of 3 stages which are the preparation of liquor, the impregnation of the biomass and the pretreatment of the biomass impregnated by steam explosion.
    Prior art
    Lignocellulosic biomass represents one of the most abundant renewable resources on earth. The substrates considered are very varied, they concern both woody substrates such as different woods (hardwoods and conifers), co-products from agriculture (wheat straw, corn cobs, etc.) or other industries. food, paper, etc.
    The biochemical transformation process of lignocellulosic into 2G sweet juices notably includes a pretreatment step and an enzymatic hydrolysis step with an enzymatic cocktail. These methods also most often include an impregnation step before the pretreatment. The sugary juices from the hydrolysis are then treated, for example by fermentation, and the process also includes separation steps and / or a purification step of the final product.
    Lignocellulosic biomass is composed of three main polymers: cellulose (35 to 50%), which is a polysaccharide essentially made up of hexoses; hemicellulose (20 to 30%), which is a polysaccharide essentially consisting of pentoses; and lignin (15 to 25%), which is a polymer of complex structure and of high molecular weight, composed of aromatic alcohols linked by ether bonds. These different molecules are responsible for the intrinsic properties of the plant wall and are organized into a complex tangle.
    Among the three basic polymers that integrate lignocellulosic biomass, cellulose and hemicellulose are those that allow the production of 2G sweet juices.
    Most often, hemicellulose is mainly broken down into sugar during pretreatment and cellulose is converted to glucose by enzymatic hydrolysis. However, access to raw cellulose remains difficult for enzymes to access, hence the need for pretreatment. This pretreatment makes it possible to modify the physicochemical properties of lignocellulose in order to improve the accessibility of cellulose to enzymes and its reactivity to enzymatic hydrolysis.
    One of the most effective pretreatments is the steam explosion which allows almost complete hydrolysis of hemicellulose and a significant improvement in the accessibility and reactivity of cellulose to enzymes. This pretreatment can be preceded by other treatment (s).
    The patents US-8057639 and US-8512512 propose a process comprising a first step of hydrolysis of hemicellulose to C5 sugars under mild conditions thus preserving them from their degradation. This step is carried out in a first reactor at a pressure of 1.5 bar or more by steam injection, at a temperature of 110 ° C plus, and possibly in the presence of weak acid. After this step, washing is carried out to extract and recover the C5 sugar juices before sending the remaining biomass, enriched in cellulose and lignin, in a second step (second reactor) where the steam explosion takes place. This second reactor operates at a higher pressure than the first reactor with an injection of steam at high pressure which causes a sudden expansion of the biomass (steam explosion).
    Patent application US-2012/0104313 also proposes a treatment step prior to a steam explosion by contact of the biomass with water or steam at 100-210 ° C for 1 min-24h. After separation of the liquid phase enriched in hemicellulose, the solid is then transferred to the steam explosion step.
    Patent EP-2610346 describes a process for treating lignocellulosic biomass in 4 stages: treatment in a liquid at a temperature of 100-150 ° C., followed by separation of the liquid / solid, followed by pretreatment of the solid part obtained at 100-210 ° C in the presence of water or steam for 1 min-24h and ending with a liquid / solid separation.
    Many patents offer different solutions to improve the pretreatment by dissolving the hemicellulose leading to better reactivity of the biomass to steam explosion: impregnation at high temperature, impregnation under pressure, presence of acid, multiplication of stages under the same or different conditions.
    Patent application WO-2013/141776 describes, in the paper industry, a method of impregnation in a vertical device (impregnator) including one containing basic impregnation liquor, thus defining a first zone in which the impregnation is carried out . The lignocellulosic material is received at the bottom of the impregnator, it is transferred to the top of the impregnator by means of 2 transfer screws. When transferred to the second zone of the impregnator located above the liquid level, the biomass drips and the liquid falls back into the first zone. In this configuration, the liquid level is controlled by the supply of basic liquor.
    In the improved arrangement, liquid is extracted at the bottom of the impregnator, is filtered and is recycled at the top of the impregnator, so as to create a counter-current opposite to the direction of advance of the biomass, which allows to evacuate the biomass of impurities (sand ...) which otherwise settle at the bottom of the impregnator. The liquid loops through a filtration system and fresh liquor can be added.
    There is proposed in the present application a method using the impregnator described in application WO-2013/141776, which is suitable for continuous use and on an industrial scale with regulation of the operating conditions. The process according to the invention, and the associated installation, is particularly applicable to processes for the production of sugary juices, or even alcohols, from lignocellulosic biomass.
    This process is simpler, less expensive than the processes of the prior art in the field of production of sugary juices. It operates at moderate temperature and atmospheric pressure, and preferably in a single impregnation step.
    Summary of the invention
    More specifically, the process according to the invention relates to a continuous process for the treatment of a lignocellulosic biomass for the production of sugary juices, operated before an enzymatic hydrolysis, a process comprising
    1) a first transfer zone of the crushed biomass towards the first zone of the impregnation step, said zones being separated by a biomass plug preventing the ascent of liquid from said first zone to the transfer zone,
    2) an impregnation step at atmospheric pressure carried out in 2 superimposed zones operating at a temperature of 10-95 ° C, the residence time of the biomass in said step being 1mn-60mn, and
    - said first zone receives the pressed biomass from the transfer zone and it contains an acid impregnating liquor at pH between 0.1 and 7 and
    - Said biomass is transferred to a second zone, located above said first zone, in which the impregnated biomass drips, the resulting wet biomass having a dry matter content of between 15% w / w and 40% w / w, and the separate liquor flows into said first zone,
    3) a second wet biomass transfer zone during the steam explosion stage,
    said transfer zone being arranged in an enclosure separated on the one hand from the zones of said impregnation step and on the other hand from the zones of the vapor explosion step,
    the second impregnation zone and the reactor of the steam explosion stage being separated in leaktight manner by a plug of biomass, and
    - in said transfer zone, the wet biomass is pressed so as to increase the dry matter content of the biomass to 40% by weight or more, and all or part of the resulting liquor is preferably sent to the preparation stage liquor,
    4) a steam explosion step comprising
    - a cooking zone for 1-30mn of biomass by steam injection with a specific steam consumption of between 0.05 and 10 ton / ton of dry matter of biomass entering this zone, said zone being at a temperature of 150 250 ° C. and a pressure of 0.5-4 MPa,
    - then a relaxation zone for the biomass from the cooking zone,
    - then an area for the separation of steam from biomass,
    5) a step of preparing the acid liquor
    - which receives liquor extracted from the transfer zone and / or the first impregnation zone,
    - which receives acid and / or water inputs determined so as to maintain the pH at the input of the first impregnation zone at a value between 0.1 and 7
    - and said liquor is introduced into the first impregnation zone.
    Preferably, in the method according to the invention, the impregnation step is carried out in a single step.
    Advantageously,
    - the impregnation step is carried out in 2 zones arranged vertically one above the other and along the same axis, separated so as to let the liquor pass from the second zone to the first zone and so as to retaining the biomass in the second zone, the level of the liquid in the first zone ensuring the separation between said 2 zones,
    - Said biomass is transferred by means of screws from said first zone into said second zone.
    From said second zone, part of the liquor is separated from the impregnated biomass, preferably a part of the liquor from the impregnated biomass drips (is separated by drainage) in said first zone.
    It is preferable to keep the liquor level almost constant by adding acid liquor. Generally, the acid liquor is only a solution of sulfuric acid.
    Preferably, the acid liquor has a pH of between 0.1 and 2.
    In one embodiment of the step of preparing the acid liquor receives liquor extracted from the transfer zone and optionally from the liquor from the first impregnation zone. In another mode, the step of preparing the acid liquor receives liquor from the first impregnation zone and optionally liquor extracted from the transfer zone. In a preferred embodiment, the step for preparing the acid liquor receives liquor from the first impregnation zone and liquor extracted from the transfer zone.
    In general, the liquor preparation stage does not receive the separated liquor in or after the steam explosion stage.
    Generally, the cooking zone is a horizontal tubular reactor, and provided with one or more screws transporting the biomass from the transfer zone upstream to the expansion zone downstream. By "horizontal", it is understood that there is a slight inclination allowing the flow of the liquid.
    Preferably, at least part of the biomass resulting from the steam explosion step is subjected to enzymatic hydrolysis and sweet juices are obtained.
    Preferably, at least part of the sweet juices is subjected to alcoholic fermentation, generally with production of ethanol.
    The invention also relates to an installation for the continuous treatment of a lignocellulosic biomass before enzymatic hydrolysis, comprising:
    1) a transfer zone with pressing of the crushed biomass towards the first zone of an impregnation reactor, said zones being separated by a biomass plug preventing the ascent of liquid from said first zone to the transfer zone,
    2) an impregnation reactor comprising 2 superimposed zones, the second zone being located above the first zone
    - said first zone containing an acid liquor and being provided with an inlet opening for the pressed biomass originating from the transfer zone,
    - the reactor being provided with a screw transferring said biomass from said opening opening in the first zone to the opening opening in the second zone,
    - the second zone located above the liquid of the first zone being provided with grid (s) allowing the liquid to flow from the second zone into the first zone and retaining the wet biomass in the second zone,
    3) a transfer zone with pressing of the wet biomass to the steam explosion reactor,
    said transfer zone being arranged in an enclosure separated on the one hand from the zones of said impregnation step and on the other hand from the zones of the vapor explosion step,
    - the second impregnation zone and the reactor of the steam explosion step being separated by a plug of pressed biomass so as to increase the dry matter content of the biomass to 40% by weight or more, said plug preventing the ascent of liquid from the vapor explosion zone to the transfer zone, and
    - said transfer zone, being provided with a line for drawing off the spent liquor separated from the wet biomass during pressing,
    4) a steam explosion zone comprising a screw for transferring the biomass through the following successive zones:
    - a biomass cooking zone provided with a pipe for bringing the pressed biomass coming from the transfer zone and a steam injection pipe,
    - a biomass relaxation zone from the cooking zone,
    - an area for the separation of steam from biomass,
    5) an acid liquor preparation area with
    - a pipe bringing the spent liquor drawn from the transfer zone to the explosion and / or a pipe bringing the spent liquor withdrawn from the first impregnation zone,
    - a pipe bringing the acid and / or a pipe bringing the water
    - a recycling line in the first impregnation zone of said prepared acid liquor,
    - a stirring system and possibly a heating means.
    detailed description
    The process according to the invention is a continuous process for the treatment of a lignocellulosic biomass before enzymatic hydrolysis.
    It is part of processes aimed at producing second generation sugars from which numerous biochemical pathways make it possible to obtain oxygenated molecules (for example alcohols such as ethanol, butanol ...).
    Thus, the present application relates to an integrated acid impregnation process followed by a steam explosion pretreatment with recycling and regulation of the acid impregnation liquor.
    This process is compatible with the production processes of 2G sugars (that is to say obtained from lignocellulosic biomass) or more broadly from bio-sourced molecules (that is to say from natural substrates or derived from natural substrates).
    Biomass and the transfer area
    Depending on the biomass (straw, wood, etc.), a grinding stage is necessary in order to have a particle size compatible with the technological means and the operating conditions of the stages. For this, a simple shredding may be sufficient but grinding with or without refining may be required.
    Generally, the crushed biomass has a particle size (the largest size) of at most 300mm. Most often, the crushing of the straws is done with grids of 5 to 100 mm and the wood is shredded into parallelepiped plates with a length between 20 and 160 mm, a width between 10 and 100 mm and a thickness between 2 and 20 mm.
    The crushed biomass is brought to the first zone of the impregnation stage via a transfer zone. Advantageously, these zones are separated by a biomass plug which prevents the ascent of liquid from said first zone towards the transfer zone or even further upstream.
    The transfer zones with pressing described in the text are provided with screws, a conical compression zone allowing the formation of a sealed cap; a perforated zone allows the exit of liquor.
    One means usually used for this purpose is a screw called a "sealing screw" or "plug screw" known to those skilled in the art.
    This screw has a conical part, said conical part being connected to the bottom of the first impregnation zone. The biomass plug is created at the end of this conical part just before entering the first zone.
    This screw thus performs a double function: on the one hand, the continuous introduction of the biomass into the impregnation reactor, and on the other hand the formation of a plug to seal and prevent leaks from liquor from the impregnation reactor to the screw and upstream of the screw.
    The impregnation step
    The impregnation is carried out under atmospheric pressure and at a temperature of 10-95 ° C. The residence time of the biomass in the first impregnation zone is usually 1mn-60mn, preferably at least 2mn, preferably at least 5mn, preferably at most 45mn, and most often 2-35mn. Preferably, it is carried out in a single step.
    The step is carried out in an impregnation reactor (or impregnator) of tubular shape and vertical or inclined at an angle less than 60 ° relative to the vertical. This reactor has 2 superimposed zones, preferably located on the same axis. The bottom zone is called the first zone and receives, by an opening, the pressed biomass from the transfer zone. The area above (top area) is called the second area, it receives the biomass from the first area.
    The reactor is equipped with one or more screws which transfer (s) the biomass from its entry into the impregnator (bottom of the first zone) to the outlet opening of the impregnator (top of the second zone).
    The first zone (therefore the zone where the impregnation takes place) corresponds to the space filled by the impregnation liquor. The second zone does not contain a continuous liquid phase. It is particularly advantageous to maintain a constant distribution between the first zone and the second zone. To do this, the reactor is equipped with a detection system (level sensor), preferably with a liquor level regulation system, making it possible to guarantee filling at the desired level.
    The impregnation liquor is an acidic aqueous solution and has a pH of 0.1 to 7.0, reference 0.1 to 6, or better 0.1 to 2, and a temperature of 10-95 ° C. The acid is usually sulfuric acid. This type of liquor is well known to the person skilled in the art and any acid usually used for impregnation is suitable. The amount of acid and the temperature of the liquor are usually set. The means for obtaining and maintaining the temperature are known to those skilled in the art.
    The effect of compression of the biomass during the formation of the plug (at the level of the transfer screw) and decompression at the inlet of the first zone filled with liquor makes it possible to better fill the biomass (sponge effect). The biomass is transferred through the first zone where it is impregnated to the second zone located above the level of the liquor.
    In the second zone, part of the impregnated liquor separates from the impregnated biomass by draining during the ascent into the second zone, the drained liquor falling back into the first zone.
    Preferably, the second zone is provided with grid (s) retaining the wet biomass in the second zone., Grid which therefore lets the liquid flow from the second zone into the first zone.
    At the outlet of the second zone and of the reactor, the impregnated and drained biomass is recovered and contains little or no free water. Its dry matter content generally varies between 15 and 40% by weight.
    The separated liquor, often called spent liquor, is found in the liquid of the first impregnation zone.
    The impregnator is equipped with one or more lines for supplying liquor from the liquor preparation area and one or more lines for withdrawing liquor. Said liquor inlet and outlet pipes are generally installed opposite the bottom and the top of the first zone, which makes it possible to operate in co-current or countercurrent recycling.
    The preparation of the impregnation liquor
    As a result of the impregnation, there is a loss of liquor and acidity. It is therefore necessary to regularly add fresh acid liquor.
    These additions make it possible to precisely regulate the level of liquor in the impregnation reactor.
    The preparation of liqueur is also a step that allows you to regulate its operating parameters such as, for example, temperature, pH or any other characteristic. The correct acid concentration is adjusted by adding acid and / or water.
    It also makes it possible to produce a homogeneous liquor.
    This step is carried out in a liquor preparation area.
    Various devices can be used, such as, for example, a mixing tank with a stirring system or a mixer (preferably a static mixer).
    Preferably, the device is equipped with pH and flow measurement sensors for water, acid, spent liquor and prepared liquor ...
    Furthermore, the impregnator is advantageously equipped with a level measurement sensor.
    All of these sensors make it possible to set up a regulation which balances the flow rates and the acidities so as to have a stable continuous walking under the desired conditions.
    The apparatus and / or the impregnator is equipped to carry out the heating by means, for example, of a double envelope, of coils and / or of exchangers arranged on the recirculation loop (described below) next to or directly on said said devices (tank, mixer ...).
    The apparatus used for the preparation of the liquor is connected to the impregnator by one or more pipes carrying the liquor.
    The liquor can thus be prepared with the appropriate concentration and flow rate which make it possible to obtain the determined pH (or any other characteristic) which may be the setpoint for regulation ... We will not detail the means of regulation that the skilled person knows.
    Generally, the acid liquor preparation area is provided
    - a pipe bringing the spent liquor drawn from the second transfer zone to the vapor explosion zone and / or a pipe bringing the spent liquor withdrawn from the first impregnation zone,
    - a pipe bringing the acid and / or a pipe bringing the water
    - a recycling line in the first impregnation zone of said prepared acid liquor,
    - a stirring system and possibly a heating means.
    Examples of the recirculation loop are shown below.
    Simple recirculation loop called "pump-around" recycling
    A liquor recirculation loop can advantageously be arranged around the first zone of the impregnation step and which is commonly called "pump-around" because it is a question of withdrawing and recycling in the same zone.
    Liquor is drawn off near the liquid level of the first zone after separation of the biomass. This liquor is drawn off at a place where the concentration of spent liquor is high, so that, in the liquor preparation zone, its characteristics are adjusted to those of the fresh liquor.
    Before returning, the spent liquor goes through the preparation stage where it is added with acid and / or water in the appropriate proportions.
    This arrangement makes it possible to considerably improve the homogeneity of the liquor in the first impregnation zone, to have more effective contact between the biomass and the liquor and to be able to have a higher temperature in the first zone. In this case, the advantage is to have reduced differences between the characteristics of fresh liquors and used liquors.
    There are two possibilities for reinjection: co-current (bottom injection and top racking) or countercurrent (top injection and bottom racking). This loop makes it possible to have a better homogeneity and stability of the liquor, a better contact of the liquor with the biomass and also makes it possible to regulate the level of liquor of the first impregnation zone.
    The characteristics of the liquor entering the preparation stage are measured using sensors (pH, flow rate, etc.) and the quantities of water and / or acid to be added are determined by the control system to reach the (the) set value (s), for example the pH of the liquor to be recycled in the first impregnation zone.
    Description of the figures which will be followed from the following references:
    Figure 1: simple pump-around recycling (co-current): crushed biomass: 1 st zone / transfer step
    3a: impregnator, first zone
    3b: impregnator, second zone: liquor withdrawn from the impregnator for co-current pump-around recycling: liquor injected into the impregnator for co-current pump-around recycling: apparatus (tank) for preparing liquor
    7: make-up of water in the liquor preparation tank: make-up of acid in the liquor preparation tank: second zone / transfer step: downstream of the impregnation process (pre-treatment by steam explosion).
    Figure 2: simple recycling after pressing downstream of the impregnation
    1: crushed biomass: first zone / transfer stage
    3a: impregnator, first zone
    3b: impregnator, second zone: liquor injected into the impregnator for recycling in co-current pump-around
    6: liquor preparation tank: line for adding water to the liquor preparation tank: line for adding acid to the liquor preparation tank: second zone / transfer step: downstream of the process impregnation (pre-treatment by steam explosion): liquor drawn off by pressing (pressat) after impregnation in the second transfer zone
    Figure 3: double recycling in pump-around (co-current) and in pressat: crushed biomass: first zone / transfer step
    3a: impregnator, first zone
    3b: impregnator, second zone: liquor injected into the impregnator for co-current pump-around recycling: liquor withdrawn from the impregnator for co-current pump-around recycling: liquor preparation tank: make-up water the liquor preparation tank: line for adding acid to the liquor preparation tank: second zone / transfer step: downstream of the impregnation process (pre-treatment by steam explosion): liquor drawn off by pressing (pressat) after impregnation in the second transfer zone.
    Figure 1 illustrates how this loop works.
    The crushed biomass is introduced via line 1 into the process and transferred (first transfer zone 2) into the impregnator 3, and more precisely into the first zone of the impregnator 3a. This zone contains the liquor supplied via line 4 and which comes from the apparatus (step) 6 for preparing the liquor. This device receives via line 5, the liquor coming from the second zone 3b of the impregnator and which has been separated from the biomass, and is provided with lines 7 and 8 for the addition of water and acid respectively. The wet biomass obtained after separation of the liquid is transferred (second transfer zone 9) to the next stage of the process, which is most often a stage of pre-treatment by steam explosion, carried out for example in zone 10.
    Simple recirculation loop with one or more other downstream liquid streams
    Other liquid streams separated after the impregnation step (or after the impregnator), and more precisely after the second zone of this step, can also be recycled into impregnation after passing through the step (the apparatus) of preparation of liqueur. Advantageously, the characteristics of the flow are measured by sensors (flow rate, pH, etc.) before the introduction of the flow in the preparation step. The regulation of the device allows the addition of water and / or acid in the right proportions to prepare the liquor with the appropriate characteristics. Preferably, said flow is the pressate (liquid from the wet biomass transfer zone in the steam explosion step). Indeed, this stream is a spent liquor which still contains acid which can therefore be recovered.
    The operation of a liquid recycling downstream of the impregnation is as follows (with reference to FIG. 2): the description and the commented references for FIG. 1 will not be repeated when they are identical.
    In FIG. 2, a line 11 which brings the pressat to the liquor preparation stage. The pressate comes from the second transfer zone 9 (transfer of wet biomass to the steam explosion zone).
    On the other hand, in this arrangement of FIG. 2, the spent liquor separated from the biomass in the second zone of the impregnator is not sent in the stage of preparation of the liquor.
    This arrangement is preferably used when there is little difference between the fresh liquor entering the first zone and the spent liquor separated from the biomass in the pressate (or more generally in this other flow).
    Recirculation loop known as double recycling
    It combines the 2 previous recycling loops to benefit from their cumulative advantages.
    Figure 3 illustrates the operation of double recycling. We will not repeat the descriptions of the previous figures, which are identical.
    Thus, in FIGS. 1 and 3, the spent liquor 5 from the first zone of the impregnator makes a loop passing through the zone for preparing liquor. This recycling can be done in co-current or against the current of the biomass circulation in the first zone of the impregnator.
    Similarly, the downstream liquor 11 (which is for example the pressate from the second transfer) is sent to the preparation zone. Thus, the preparation area receives two (or more) spent liquors and allows them to be mixed.
    The aforementioned sensors send the information necessary to determine the adequate amounts of water and acid to be added to obtain a recycled liquor having the desired pH and flow rate for the first zone of the impregnator.
    The liquor preparation step can therefore be carried out in different ways:
    - without sampling and recycling of liquor from the impregnator or from another process zone; this provision does not bring any particular advantage,
    - with withdrawal of liquor from the impregnator and recycling of liquor in the first zone of the impregnator;
    - with the removal of one or more liquids present downstream of the impregnation (such as the pressat) and recycling in the first zone of the impregnator; this provision is advantageous, in particular in cases where there is little difference in characteristic between the downstream liquor and the fresh liquor,
    - with double recycling, that is to say with withdrawal of liquor from the impregnator and recycling of liquor in the first zone of the impregnator and also withdrawal of one or more liquids present downstream of the impregnation and recycling in the first zone the impregnator. This arrangement is widely preferred.
    Transfer area with pressing to the steam explosion step
    The wet biomass from the second zone of the impregnation stage is transferred continuously to the steam explosion stage via a second transfer zone.
    This zone is separate from the impregnation zones and is not arranged within the enclosure of either of the impregnation zones. For example, in the case of an impregnator having 2 zones (impregnation and drainage), the transfer zone is outside the impregnator.
    This area is also separate from the steam explosion areas.
    In the same way as in the first transfer zone bringing the biomass to the impregnation stage, the second impregnation zone and the reactor where the steam explosion stage takes place are separated by a biomass plug. . Said cap prevents the liquid from rising from the first zone of the vapor explosion to the transfer zone or more upstream.
    This seal is ensured in the transfer zone between said second zone of the impregnation stage and the first zone of the vapor explosion stage.
    One means usually used for this purpose is a screw called a "plug screw" known to those skilled in the art. The conical part of the screw is here connected to the first vapor explosion zone. The non-conical part is connected to said second zone.
    The formation of a biomass plug seals the pressure of the steam explosion reactor, thereby preventing dangerous vapor leaks.
    In said transfer zone, the wet biomass is pressed so as to increase the DM content of the biomass. The dry matter content of the biomass is generally at least 40% by weight, preferably it is greater than 40% by weight and even more preferably it is from 40% by weight to 70% by weight.
    The transfer area is also provided with a line for drawing off the spent liquor (called pressat) separated from the wet biomass during pressing.
    The spent liquor is advantageously recycled in the impregnation step, as described above.
    It should be noted that the drained biomass does not undergo mechanical treatment before hydrolysis to reduce the sizes.
    The steam explosion step performed in a steam explosion zone
    It involves :
    - a cooking zone for 1-30mn of biomass by steam injection with a specific steam consumption of 0.05-10 ton / ton of dry biomass material, said zone being at a temperature of 150-250 ° C and a pressure of 0.5-4 MPa,
    - then a relaxation zone for the biomass from the cooking zone
    - then an area for separating the steam from the biomass.
    The recovered steam is advantageously recycled after compression in the steam explosion stage, or is recycled on site utilities.
    It is carried out in a horizontal tubular reactor (i.e. which can be very slightly inclined for the flow of the liquid).
    The biomass cooking zone is provided with a pipe for bringing the pressed biomass from the transfer zone and with a steam injection pipe. Cooking is carried out at high temperature and under pressure. This pressurization is ensured by steam injection so as to reach a pressure of 0.5-4 MPa. The cooking temperature is generally 150-250 ° C. Preferably, the conditions are set so that the cooking time is limited to 1-30mn.
    The reactor is equipped with a biomass transfer screw through the successive zones. The screw ensures the transport of the biomass continuously, the speed of the screw being adjusted to meet the residence time conditions.
    At the end of the screw (at the end of the reactor), the biomass is very quickly entrained by the steam towards an expansion zone in a line called "blowline" which has a reduced diameter compared to the cooking zone.
    The expansion zone includes a line in which the biomass circulates and passes through a section restriction member then, after having crossed the restriction, undergoes a sudden expansion.
    The blowline has a section restriction member which can be an orifice or an adjustable opening valve (diaphragm valve for example) allowing a small passage section. At the level of this restriction, the biomass arrives with a very high transport speed, and it undergoes a rapid and significant variation in pressure, then a sudden expansion after having crossed the restriction, which destructures the cooked biomass. That’s why we’re talking about a steam explosion.
    This restriction fixes the steam flow and therefore the specific steam consumption (steam flow / dry biomass flow). Generally this specific consumption of steam is 0.05-10 ton / ton of dry matter.
    Once the expansion zone has passed, the biomass is entrained by steam in the rest of the "blowline" which has a diameter larger than the restriction (or which regains its diameter upstream of the restriction) and which brings the biomass up to 'to a vapor separation zone, for example by a cyclone.
    The exploded biomass from the separation zone now has sufficient accessibility of cellulose to enzymes to be treated by enzymatic hydrolysis for the production of 2G sugars.
    The conditions of the enzymatic hydrolysis and of the consecutive or simultaneous fermentation are adapted to the desired products and are known to the skilled person.
    This process according to the invention finds a particularly advantageous application in a process for the preparation of sugars from lignocellulosic biomass and in the process for producing ethanol from said sweet juices.
    Such methods are known. A process for the preparation of sugars from lignocellulosic biomass comprises a pretreatment, which is advantageously a steam explosion, followed by an enzymatic hydrolysis. The process for producing ethanol from sugars further comprises an alcoholic fermentation of said sugars.
    In a process according to the invention, at least part of the biomass resulting from the steam explosion step is subjected to an enzymatic hydrolysis and sweet juices are obtained. Preferably, said biomass is introduced without an intermediate mechanical step into the enzymatic hydrolysis reactor.
    In a process according to the invention, at least part of the biomass resulting from the steam explosion step is subjected to an enzymatic hydrolysis, sugar juices are obtained and at least part of sugar sugars is subjected to alcoholic fermentation.
    权利要求:
    Claims (15)
    [1" id="c-fr-0001]
    1. Continuous process for the treatment of lignocellulosic biomass for the production of sugary juices, operated before an enzymatic hydrolysis, process comprising
    1) a first transfer zone of the crushed biomass towards the first zone of the impregnation step, said zones being separated by a biomass plug preventing the ascent of liquid from said first zone to the transfer zone,
    [2" id="c-fr-0002]
    2) an impregnation step at atmospheric pressure carried out in 2 superimposed zones operating at a temperature of 10-95 ° C, the residence time of the biomass in said step being 1 min-60 min, and
    - said first zone receives the pressed biomass from the transfer zone and it contains an acid impregnating liquor at pH between 0.1 and 7 and
    - Said biomass is transferred to a second zone, located above said first zone, in which the impregnated biomass drips, the resulting wet biomass having a dry matter content of between 15% w / w and 40% w / w, and the separate liquor flows into said first zone,
    [3" id="c-fr-0003]
    3) a second wet biomass transfer zone during the steam explosion stage,
    said transfer zone being arranged in an enclosure separated on the one hand from the zones of said impregnation step and on the other hand from the zones of the vapor explosion step,
    the second impregnation zone and the reactor of the steam explosion stage being separated in leaktight manner by a plug of biomass, and
    - in said transfer zone, the wet biomass is pressed so as to increase the dry matter content of the biomass to 40% by weight or more, and all or part of the resulting liquor is preferably sent to the preparation stage liquor,
    [4" id="c-fr-0004]
    4) a steam explosion step comprising
    - a cooking zone for 1-30mn of biomass by steam injection with a specific steam consumption of between 0.05 and 10 ton / ton of dry matter of biomass entering this zone, said zone being at a temperature of 150 250 ° C. and a pressure of 0.5-4 MPa,
    - then a relaxation zone for the biomass from the cooking zone,
    - then an area for the separation of steam from biomass,
    [5" id="c-fr-0005]
    5) a step of preparing the acid liquor
    - which receives liquor extracted from the transfer zone and / or the first impregnation zone,
    - which receives acid and / or water inputs determined so as to maintain the pH at the input of the first impregnation zone at a value between 0.1 and 7
    - and said liquor is introduced into the first impregnation zone.
    2. Method according to claim 1 wherein said impregnation step is carried out in a single step.
    3. Method according to one of the preceding claims wherein
    - the impregnation step is carried out in 2 zones arranged vertically one above the other and along the same axis, separated so as to let the liquor pass from the second zone to the first zone and so as to retaining the biomass in the second zone, the level of the liquid in the first zone ensuring the separation between said 2 zones,
    - Said biomass is transferred by means of screws from said first zone into said second zone.
    4. Method according to one of the preceding claims wherein the level of liquor is kept almost constant by adding acid liquor.
    5. Method according to one of the preceding claims wherein the acid liquor is only a solution of sulfuric acid.
    [0006]
    6. Method according to one of the preceding claims wherein the acid liquor has a pH between 0.1 and 2.
    [0007]
    7. Method according to one of the preceding claims wherein said step of preparing the acidic liquor receives liquor extracted from the transfer zone and optionally liquor from the first impregnation zone.
    [0008]
    8. Method according to one of the preceding claims wherein said step of preparing the acidic liquor receives liquor from the first impregnation zone and optionally liquor extracted from the second transfer zone.
    [0009]
    9. Method according to one of the preceding claims in which in said wet biomass transfer zone the dry matter content of the biomass after pressing is between 40% and 70% by weight, and preferably is greater than 40% by weight.
    [0010]
    10. Method according to one of the preceding claims, in which the cooking zone is a horizontal tubular reactor, and provided with one or more screws transporting the biomass from the transfer zone upstream to the expansion zone downstream.
    [0011]
    11. Method according to one of the preceding claims wherein the crushed biomass has a size of at most 300mm.
    [0012]
    12. Method according to one of the preceding claims wherein at least part of the biomass from the steam explosion step is subjected to enzymatic hydrolysis and sweet juices are obtained.
    [0013]
    13. The method of claim 12 wherein at least part of the sweet juices is subjected to alcoholic fermentation.
    [0014]
    14. Installation for continuous treatment of lignocellulosic biomass before enzymatic hydrolysis, comprising:
    1) a first transfer zone with pressing of the crushed biomass towards the first zone of an impregnation reactor, said zones being separated by a biomass plug preventing the ascent of liquid from said first zone to the transfer zone,
    2) an impregnation reactor comprising 2 superimposed zones, the second zone being located above the first zone
    - said first zone containing an acid liquor and being provided with an inlet opening for the pressed biomass originating from the transfer zone,
    - the reactor being provided with a screw transferring said biomass from said opening opening in the first zone to the opening opening in the second zone,
    - the second zone located above the liquid of the first zone being provided with grid (s) allowing the liquid to flow from the second zone into the first zone and retaining the wet biomass in the second zone,
    3) a second transfer zone with pressing of the wet biomass to the steam explosion reactor,
    said transfer zone being arranged in an enclosure separated on the one hand from the zones of said impregnation step and on the other hand from the zones of the vapor explosion step,
    - the second impregnation zone and the reactor of the steam explosion stage being separated by a plug of pressed biomass so as to increase the dry matter content of the biomass to 40% by weight or more, said plug preventing the ascent of liquid from said first zone to the transfer zone, and
    - said transfer zone, being provided with a line for drawing off the spent liquor separated from the wet biomass during pressing,
    4) a steam explosion zone comprising a screw for transferring the biomass through the following successive zones:
    5 - a biomass cooking zone provided with a pipe for bringing the pressed biomass coming from the transfer zone and a steam injection pipe,
    - a biomass relaxation zone from the cooking zone,
    - an area for the separation of steam from biomass,
    5) an acid liquor preparation area with
    10 - a pipe bringing the spent liquor drawn from the second transfer zone to the explosion and / or a pipe bringing the spent liquor withdrawn from the first impregnation zone,
    - a pipe bringing the acid and / or a pipe bringing the water
    - a recycling line in the first impregnation zone of said acid liquor
    [0015]
    15 prepared,
    - a stirring system and possibly a heating means.
    1/1
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1656829A|FR3053969B1|2016-07-18|2016-07-18|PROCESS OF TREATING LIGNOCELLULOSIC BIOMASS BY IMPREGNATION AND EXPLOSION WITH STEAM|
    FR1656829|2016-07-18|FR1656829A| FR3053969B1|2016-07-18|2016-07-18|PROCESS OF TREATING LIGNOCELLULOSIC BIOMASS BY IMPREGNATION AND EXPLOSION WITH STEAM|
    US16/318,581| US11236403B2|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    ES17737286T| ES2811353T3|2016-07-18|2017-07-11|Procedure for treating lignocellulosic biomass by impregnation and steam explosion|
    RS20201006A| RS60763B1|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    AU2017299081A| AU2017299081B2|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    SI201730389T| SI3484945T1|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    DK17737286.9T| DK3484945T3|2016-07-18|2017-07-11|PROCEDURE FOR TREATING A LIGNOCELLULOSE BIOMASS BY IMPREGNATION AND STEAM EXPLOSION|
    PCT/EP2017/067468| WO2018015227A1|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    PL17737286T| PL3484945T3|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    CA3030096A| CA3030096A1|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
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    HUE17737286A| HUE051670T2|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    LTEP17737286.9T| LT3484945T|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    EP17737286.9A| EP3484945B1|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    MX2019000320A| MX2019000320A|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion.|
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    BR112019000349-5A| BR112019000349A2|2016-07-18|2017-07-11|steam impregnation and explosion lignocellulosic biomass treatment process|
    PT177372869T| PT3484945T|2016-07-18|2017-07-11|Method for treating lignocellulosic biomass by impregnation and steam explosion|
    ZA2018/08547A| ZA201808547B|2016-07-18|2018-12-19|Method for treating lignocellulosic biomass by impregnation and steam explosion|
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