METHOD FOR TREATING LIGNOCELLULOSIC BIOMASS

Abstract

The invention relates to a process for treating a lignocellulosic biomass, with: a. Pretreatment of the biomass via at least one cooking or steam explosion operation, so as to obtain a pretreated substrate, b. Liquid/solid separation on at least a portion of the pretreated substrate, comprising two successive substeps: an upstream substep b1 of contacting the solid/liquid mixture performed with a continuous mixer (M) using a mixing fluid, a downstream sub-step b2 of extraction/washing performed with a continuous filter, using a washing fluid, to obtain a solid phase enriched in solid and a plurality of liquid phases enriched in liquid, with at least partial recycling of a liquid phase extracted from the filter at the inlet of the mixer as a mixing fluid.

Claims

1. Process for treating a lignocellulosic biomass, said process comprising at least the following step: a. Pretreatment of the biomass via at least one cooking or steam explosion operation, so as to obtain a pretreated substrate, characterized in that it also comprises at least one step of: b. Liquid/solid separation on at least a portion of the pretreated substrate obtained on conclusion of step a or on conclusion of an additional step of treatment of said substrate after step a, said separation step comprising two successive substeps: an upstream substep b1 of contacting the solid/liquid mixture performed with a continuous mixer (M) using a mixing fluid, optionally preceofd by a pump, and a downstream sub-step b2 of extraction/washing performed with a continuous filter, notably a belt filter (F), using a washing fluid, to obtain a solid phase enriched in solid and a plurality of liquid phases enriched in liquid, with at least partial recycling of a liquid phase extracted from the filter at the inlet of the mixer as a mixing fluid.

2. Process according to claim 1, characterized in that the continuous filter functions counter-currentwise between the circulation of the solid/liquid mixture to be separated and the extraction/washing fluid.

3. Process according to claim 1, characterized in that the separation of the solid/liquid mixture is performed during step b on a first portion of the pretreated substrate obtained on conclusion of step a, in that a second portion of said pretreated substrate is subjected to at least one subsequent treatment step, notably hydrolysis, and in that the solid phase enriched in solid obtained in step b is also subjected to at least one subsequent treatment step, notably the same as those to which the second portion of the pretreated substrate is subjected.

4. Process according to claim 1, characterized in that it comprises a step e of enzymatic hydrolysis of the pretreated substrate ofrived from the pre-treatment step a to obtain a hydrolysate, in that the solid/liquid separation b is performed on at least a portion of said hydrolysate.

5. Process according to claim 1, characterized in that the solid/liquid separation b is performed on at least a portion, notably all, of the pretreated substrate obtained on conclusion of the pretreatment step a to obtain a solid phase enriched in solid, and in that it comprises a step e of enzymatic hydrolysis of said solid phase enriched in solid to obtain a hydrolysate.

6. Process according to claim 1, characterized in that the liquid phases enriched in liquid ofrived from the separation step b are sugary liquors, and in that said process also comprises a step c of producing enzymes and/or a step d of producing yeasts, and in that at least one of said sugary liquors is used for said production of enzymes c or of yeasts d.

7. Process according to claim 1, characterized in that it also comprises the following steps after the pretreatment step a: e. Enzymatic hydrolysis of the pretreated substrate, so as to obtain a hydrolysate including a solid material and a liquid phase containing sugars, f. Fermentation of the hydrolysate, so as to obtain a fermentation wine, the fermentation step f possibly succeeding or being concomitant with the enzymatic hydrolysis step e, g. Separation/Distillation of the fermentation wine, so as to obtain a distillation product in the form of an alcohol, a solvent or another biobased molecule, and vinasses, step b being performed on at least a portion of the products obtained after the hydrolysis step e and/or fermentation step f and/or separation/distillation step g.

8. Process according to claim 1, characterized in that, in the separation step b, the extraction/washing fluid is heated before introduction into the filter (F) and/or the liquid phase extracted from the filter is recycled before its introduction into the mixer, notably to a temperature of at least 30 C., notably of not more than 90 C., notably a temperature of between 40 C. and 80 C.

9. Process according to claim 1, characterized in that, in step b, the filter is a belt filter (F) which comprises at least two, notably at least three, successive zones, with withdrawal of a liquid phase in each zone.

10. Process according to claim 1, characterized in that the liquid phase from the first and/or the second zone is recycled at least partly into the inlet of the mixer (M) of step b, and in that the liquid phase withdrawn from the third and/or the last zone is at least partly recycled as washing/extraction fluid for the belt filter (F).

11. Process according to claim 1, characterized in that the operating parameters of the separation steps b1 and b2 may be selected as a function of the characteristics of the solid/liquid mixture, so that the liquid phases produced extracted from the belt filter (F) have a concentration of at least 50 g of product/kg, notably at least 50 g of sugar/kg when the separation b is performed on the pretreated substrate obtained from the pre-treatment step a.

12. Installation for treating a lignocellulosic biomass, characterized in that it comprises at least: one zone for pretreatment of the biomass via at least one cooking or steam explosion operation, so as to obtain a pretreated substrate, one zone for liquid/solid separation on at least a portion of the pretreated substrate obtained at the outlet of the pretreatment zone or of an additional treatment zone of said substrate after the pretreatment zone, said separation zone comprising two subzones in series: one upstream contacting subzone comprising a continuous mixer (M) using a mixing fluid, optionally associated with an upstream pump, andone downstream extraction/washing subzone comprising a continuous filter, notably a belt filter (F), with a washing fluid, the filter preferably functioning counter-currentwise between the circulation of the solid/liquid mixture to be separated and the extraction/washing fluid, and at least partial recycling of a liquid phase extracted by the filter into the inlet of the mixer as a mixing fluid.

13. Treatment installation according to claim 1, characterized in that it envisages, in the separation zone: fluid connection means between the filter (F) and the mixer (M) to recycle at least a portion of a liquid phase extracted by the filter into the inlet of the mixer andfluid connection means for recycling another liquid phase extracted from the filter (F) as a washing fluid for said filter.

14. Treatment installation according to claim 12, characterized in that it also comprises an enzyme production zone and/or a yeast production zone, and in that it envisages a means for transferring at least one liquid phase extracted from the belt filter from the separation zone to the enzyme production zone and/or to the yeast production zone, said liquid phase being a sugary liquor.

15. The process according to claim 1 wherein said biomass is selected from wood, straw, agricultural residues, and all dedicate energy crops, notably annual or perennial plants such as miscanthus in order to produce sugars, biofuels or biobased molecules.

Description

DETAILED DESCRIPTION

[0058] The invention will be described in detail below with the aid of non-limiting examples, illustrated by the following figures:

[0059] FIG. 1: a synoptic representation of the equipment used in the context of the invention for performing step b of separating a solid/liquid mixture in a biomass treatment process;

[0060] FIGS. 2a and 2b: two different exploitations of the equipment represented in FIG. 1 according to the type of biomass used;

[0061] FIG. 3: a schematic representation (longitudinal cross section) of the mixer pertaining to the equipment represented in FIG. 1;

[0062] FIG. 4: a functional representation in block diagram form of the separation step b performed by the invention incorporated into a biomass pretreatment step according to a first variant;

[0063] FIG. 5: a functional representation in block diagram form of a whole biomass treatment process incorporating the separation step b performed by the invention according to FIG. 4;

[0064] FIGS. 6,7,8: a functional representation in block diagram form of a whole biomass treatment process incorporating the separation step b performed by the invention according to, respectively, a second, third and fourth variant.

DESCRIPTION OF THE FIGURES

[0065] The same references correspond to the same components/fluids/products on all of the figures. The figures are very schematic, are not necessarily to scale and do not represent all the components of the equipment or all the process details concerned, but only those which more particularly concern the description of the invention.

[0066] FIG. 1 thus represents the equipment developed in the context of the invention for performing the solid/liquid separation of a mixture in a lignocellulosic biomass treatment process: the mixture to be separated is first treated in a continuous mixer M such as an IMR mixer from Parimix, represented in greater detail in FIG. 3, and then with a belt filter F such as a BFR model continuous belt vacuum filter from BHS. They are both arranged substantially horizontally, at different heights, the mixer being arranged above the belt filter.

[0067] To simplify the description of this equipment, for the sake of brevity, it will be considered that the mixture to be separated is a pretreated marc from a biomass treatment process, although the separation according to the invention can be applied to other solid/liquid mixtures of such a process (as described later with the aid of FIG. 6 et seq.).

[0068] The mixer M allows repulping of the pretreated marcs with a high content of dry matter (DM) and of solids, by adding a mixing fluid and by blending obtained by the endless spiral of the mixer conveying the marc from one end to the other of the mixer. The mixer M, as detailed in FIG. 3, comprises a cylindrical body equipped with a shaftless rotating screw V, with its upstream end equipped with a metering device D which continuously measures out the mixture to be separated, which is then injected into the mixer via a feed tube or hopper A connected to the metering device. It is represented in the operating position, i.e. in a substantially horizontal plane.

[0069] In its upstream part, the cylindrical body of the mixer is equipped with mixing fluid inlet(s) e1, e2, the fluid(s) are centrifuged by the spirals, and the liquid vortex thus created meets the stream of exploded marc in the opposite direction. By means of this principle, the volume of the mixing chamber of this mixer is low, the power used is also low and the mixer as a whole is compact. Here, the mixer is equipped with electrical heating means (not shown) to heat the interior of the cylindrical body to a temperature of about 40 to 50 C., this supply of heat promoting the obtention of greater homogeneity of the mixture leaving the mixer at a constant residence time therein. The repulped marc leaving the mixer M falls by gravity onto the upstream part of the belt of the belt filter F. Separation of this marc on the belt filter F with counter-current washing makes it possible to extract liquors concentrated in sugars. The belt filter F technology is based on vacuum filtration, the principle of which is to sequentially spread the pretreated marc over an advancing belt. This porous belt makes it possible, by vacuum suction, to separate the liquids (the liquors) from the solid, forming a cake (the washed marc), which falls at the end of the belt. Washing fluid is sprayed over the belt to wash the cake which gradually forms along the belt. The liquors are partially recycled, as detailed later. They may also be pooled as a single stream.

[0070] The belt filter F has in this example 10 active vacuum zones, numbered 1 to 10 in FIG. 1, where various steps of the washing and filtration process may take place (movable and resizable zones in the filter). It may be equipped with belts of polymer such as polyurethane or silicone on the filtering belt side to limit the losses of vacuum and to improve the separation. It may be envisaged to add a partition in the top part (or any other equivalent mechanical means), just after the first zone(s), to allow better distribution of the mixture on the belt.

[0071] The various streams entering and leaving these items of equipment are now described, from upstream to downstream: the pretreated marc M0 enters the metering device D of the mixer M, while the mixing fluid is introduced into the mixer via the inlets e1, e2 (shown only in FIG. 3). The mixed marc M1 (also referred to as MoRe later) leaves the downstream end of the mixer M and falls by gravity onto the belt B of the filter F in its upstream part. The belt conveys the marc to its downstream end, with extraction under vacuum, under the belt, of three liquid phases J1, J2 and J3, which are sugary liquors of decreasing concentrations. Above the belt, in its upstream part or its central part, are introduced two extraction/washing fluids f1 and f2 via nozzles spaced apart from each other. The fluid f1 may be water, the fluid f2 is the partial or total recycling of the liquor J3.

[0072] It naturally remains within the context of the invention to extract under vacuum not three liquid phases, but more, at least the same number as there are zones in the belt filter.

[0073] The movement of the extraction/washing fluid takes place counter-currentwise relative to the circulation of the mixture on the belt. In the context of the present invention, it is in fact, in a known manner, a simulated counter-current, in the sense that there is no actual counter-current flow in each of the washing zones. The principle of the belt filter is based on tangential washing: the mixture moves here laterally, in the figure by way of example from left to right, and the washing liquid (referred to more generally hereinabove as the extraction/washing fluid) moves from the top downwards. The injection of liquid onto the mixture which is moving on the belt may take place notably either by pouring, i.e. by gravitational flow, or by spraying. The movement from the top downwards of the liquid passing through the mixture which is moving on the belt is imposed by the vacuum that is created on the belt. The filter has sequential functioning on the mixture comprising the solid phase to be extracted (also referred to as the cake), which may be represented schematically as follows: stage 1, the belt advances, stage 2, the belt stops and a vacuum is created (and, where appropriate, pressing is performed) and liquor is extracted in each of the zones, and so on. It should be noted in general that the injection of the washing liquids is performed continuously (injection takes place when the belt is advancing and when it is at rest). The counter-current is simulated by reinjection of the extracted liquor upstream of its extraction.

[0074] All or a portion of at least one of the liquors J1, J2, J3 may be recycled as mixing fluid into the mixer M.

[0075] Under the 10 zones of the porous belt of the filter F, three liquid phases denoted J1, J2 and J3 are thus extracted under partial vacuum here, while the solid phase progressively enriched in solid, the cake G, continues its course up to the downstream part of the belt, from which it is extracted after having been subjected to a press P placed at the very end of the belt, which press terminates the separation. This pressing step is optional.

[0076] The washing fluid(s) f1, f2 are heated, for example to a temperature of from 30 to 85 C. before being poured onto the top of the cake conveyed by the porous belt, via heating means with which the delivery pipes are equipped.

[0077] The stream of sugary liquor(s) which is recycled either as mixing fluid into the mixer or as washing/extraction fluid into the filter is/are also heated before reintroduction into the filter or into the mixer, also via heating means with which their delivery pipes are equipped, for example to a temperature of from 30 to 85 C.

[0078] FIG. 2a represents a first way of implementing the installation of FIG. 1 to separate the pretreated marc of a Miscanthus-based biomass: the liquor J3 is entirely recycled into the most upstream inlet, the washing extraction fluid inlet f1 of the filter F, the liquor J2 is entirely recycled into the inlet e1 of the mixer M, as a top-up to an inlet e2 of mixer fluid in the form of water. All of the liquor J1 is extracted for use/upgrading outside of this separation installation.

[0079] FIG. 2b is another way of implementing the installation of FIG. 1 to separate the pretreated marc of a straw-based biomass. The difference with FIG. 2a is that, here, a portion of the liquor J1 also is recycled as mixing fluid into the mixer with the liquor J2.

[0080] The proportion of each of the liquors J1, J2, J3 . . . extracted from the belt filter which is recycled into the mixer or into the filter may be very variable, from 0% up to 100%. It will depend on the nature of the biomass (on its solids content), on the desired water consumption, on the desired concentration of active agents (in this case of sugars), on the liquors extracted as a function of their subsequent use, in an overall biomass treatment process, according to the needs, or as independent upgrading product.

[0081] FIG. 4 represents the integration of the separation step b into a biomass pretreatment in block diagram form. The references shown have the following meaning: [0082] 1. Biomass to be treated [0083] 2. Pretreatment step [0084] 3. Stream of fluid required for the biomass pretreatment a (water, acid catalyst, steam, etc.) [0085] 4. Stream of pretreated marc, separated into two streams 4a which goes into the separation step b and 4b (which goes into the hydrolysis step as detailed later with the aid of FIG. 5) [0086] 5. Mixer used in the separation step b according to the invention [0087] 6. Mixture leaving the mixer [0088] 7. Belt filter separator used in the separation step b according to the invention [0089] 8. Washing fluid (generally water) [0090] 9. Extracted sugary liquor [0091] 10. Washed solid [0092] 11. Intermediate liquors which are returned to the belt filter and at least a portion (11a) of which is sent to the mixer

[0093] Block 2 is the first step of conditioning and pretreatment of an inlet stream of biomass 1 with one or various reagents, by placing in contact with one or more other inlet streams 3 of fluid (water, water with a chemical catalyst of acidic or basic type, oxidizing agent, steam, etc.) and optional heat treatment(s). A stream of pretreated marc 4 is obtained as outlet stream.

[0094] Block 5 thus operates substep b1 of separation b according to the invention: it is the mixer M which receives at the inlet a portion 4a of the stream of pretreated marc 4 and at least one stream of mixing liquid comprising a portion of the liquors 11a extracted from the belt filter 7 downstream of the mixer 5.

[0095] Block 7 operates the separation substep b2 with the belt filter: it receives at the inlet the stream of solid 6 which leaves the mixer from block 5 and at least one liquid washing stream 8 with recycling of a portion 11c of the liquors extracted from downstream towards the upstream of the filter and of another portion 11a towards the inlet of the mixer of block 5, a stream of washed solid 10 leaves therefrom.

[0096] FIG. 5 represents the incorporation of the separation step b according to the invention into the whole biomass treatment process according to a first variant in accordance with FIG. 4. After blocks 2, 5 and 7 already described, the new references have the following meaning: [0097] 20. Biocatalyst production step(s) which uses the sugary liquor 9 [0098] 21. Stream of fluids required for the production of biocatalysts [0099] 22. Solution containing the biocatalysts (enzymes and/or yeasts), and optionally other fluids not shown [0100] 23. Enzymatic hydrolysis step into which is introduced the other portion 4b of the pretreated marc 4 and optionally the washed marc 10 (or step of simultaneous enzymatic hydrolysis and fermentation SSF) [0101] 24. Mixture of non-hydrolysed solid and of sugars derived from the hydrolysis as a solution (or mixture of non-hydrolysed solid and of fermentation product in the case of SSF)

[0102] This figure thus shows the invention this time incorporated into the treatment process, which, beyond the pretreatment performed on the biomass, is continued by the enzymatic hydrolysis and fermentation of the marc.

[0103] The pretreated marc 4 was split into a stream 4a which is separated according to the invention as described in the preceding figure, and a stream 4b which is directed towards the enzymatic hydrolysis step 23. Optionally, the marc separated and washed 10 according to the invention may also be directed towards this step 23 with the stream 4b. (It may otherwise be upgraded differently, in the biomass treatment process or elsewhere). A stream 24 leaves therefrom, which may, depending on whether the hydrolysis takes place simultaneously with the fermentation (SSF) or not, be composed of a mixture of non-hydrolysed solid and of sugars derived from the hydrolysis (without SSF) or of a mixture of non-hydrolysed solid and of fermentation products (with SSF).

[0104] Block 20 is the step(s) of production of the biocatalysts (enzymes, yeasts) which use(s) the sugary liquor 9 derived from the separation by the belt filter of block 7 and one or more fluid streams 21 required for the production of biocatalysts (water, nutrient, other sugars, chemical products, for example for regulating the pH, etc.), this sugary liquor 9 then serving as growth/propagation substrate or as production substrate for microorganisms (fungi) producing enzymes and/or for yeasts.

[0105] In this first variant, the extracted liquor 9 is entirely used for the production of yeasts and/or enzymes. It is also possible to use it for these purposes for only a portion of the stream 9. It is also possible to upgrade all or part of this sugary liquor 9 independently of the biomass treatment process (for example upgrading it per se).

[0106] It is also possible to subject all of the pretreated marc to the separation operation according to the invention, and not only a portion thereof, and then to send all of the separated marc into the following enzymatic hydrolysis/fermentation block.

[0107] It is also possible to use directly a portion of the raw marc (i.e. of the marc at the outlet from the pretreatment step) for enzyme production and/or for yeast propagation. For the propagation of yeasts using a marc derived from the pretreatment of biomass, reference may be made, for example, to patent WO 2016/193576. For the production of enzymes using a pretreated marc, reference may be made, for example, to patent WO 2017/174378.

[0108] A stream 22 exits from block 20 containing biocatalysts (enzymes and/or yeasts), and optionally other fluids (for example: water, chemical products notably for regulating the pH, etc.), biocatalysts if produced other than on sugary liquor, nutrients, etc.), this exiting stream 22 being injected into the inlet of the enzymatic hydrolysis block 23.

[0109] Once the enzyme production has been performed, either the entire must is exploited, i.e. both the enzymes and the fungi which have produced them are exploited, or only the enzymes are exploited (in which case a prior separation/purification step must be done), to perform the enzymatic hydrolysis of the pretreated biomass.

[0110] Preferably, the enzymatic cocktail was produced by a fungus Trichoderma reesei.

[0111] As regards the production of yeasts, the yeast produced is preferably a yeast such as Saccharomyces cerevisiae which has been genetically modified to consume xylose. The stream obtained which will be exploited in the fermentation step may contain the yeasts as a whole or concentrated must; in the latter case it is referred to as a yeast cream (a prior concentration step must then be performed).

[0112] FIG. 6 proposes to incorporate the separation step b of the invention into a second variant. The new references have the following meaning: [0113] 30. Fermentation step, for example to ethanol [0114] 31. Stream of fluids required for the fermentation [0115] 32. Solution containing the fermentation product

[0116] In this instance, there is thus a block 30 for the fermentation step different from the enzymatic hydrolysis step 23, and the separation of blocks 5, 7 of the invention is inserted between these two steps: Stream 24 derived from the enzymatic hydrolysis step is separated according to the invention, and stream 9 leaving block 7 performing the separation with the belt filter is sent as an inlet stream to the fermentation block 30, which is also fed with inlet stream 31 of the fluid(s) necessary for the fermentation, such as biocatalysts (yeasts), and optionally nutrients, etc.

[0117] Stream 32 exiting the fermentation step contains the fermentation product, which can then undergo conventional separation steps, such as distillation, dehydration, solid/liquid separation (not shown) which make it possible to obtain the desired biobased molecule (in this instance ethanol as biofuel), solid residues and liquid residues also known as vinasses.

[0118] FIG. 7 proposes to incorporate the separation step b of the invention into a third variant. The new references have the following meaning: [0119] 40. hydrolysis and fermentation steps [0120] 41. Stream containing the non-hydrolysed solid and the fermentation product [0121] 42. liquid solution stream containing the fermentation product [0122] 50. Fermentation product separation step [0123] 51. Purified fermentation product stream [0124] 52. vinasse stream

[0125] Block 40 thus represents the enzymatic hydrolysis step and the fermentation step which may be separate or simultaneous, represented by a common block for the sake of clarity. Stream 41 derived from these two steps and which thus contains a portion of non-hydrolysed solid and the fermentation product is conveyed to the inlet of the separation blocks 5, 7 according to the invention. The liquid stream containing fermentation products leaving 42 from this separation feeds block 50 of the fermentation product separation step (this liquid stream thus has a different composition from stream 9 of the preceding variants, which was only a sugary liquor). At the outlet of block 50, a liquid stream of partially purified fermentation product 51 is recovered, and a vinasse stream 52 is recovered, which may optionally (dashed arrows in the figure) be recycled as replacement for the washing water 8 of the belt filter of block 7.

[0126] FIG. 8 proposes to incorporate the separation step b of the invention into a fourth variant. The new references have the following meaning: [0127] 54. medium separated from the product containing the non-hydrolysed solid and liquid [0128] 55. vinasses

[0129] In this case, the separation step b of the invention is performed after the separation step 50: stream 54 derived from the separation 50 and including a medium separated from the product containing the non-hydrolysed solid and liquid is sent into the mixer 5, the solid stream 55 leaving the belt filter of block 7 is thus vinasses extracted by washing. In this variant, the separation step 50 may be coupled to the fermentation step, which is referred to as fermentation/separation coupling, either in situ, in the fermentation reactor itself, or on another separate circuit, where the medium after separation returns in fermentation.

[0130] In all these variants, it is seen that the separation step b according to the invention can be inserted between known steps of a biomass treatment process, in this case to exploit the sugary liquors as substrates for the propagation, growth or production of enzymes of microorganisms necessary for the conversion of biomass, but also when it is desired to upgrade these sugary liquors per se.

[0131] Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. The preceding preferred specific embodiments are, therefore, to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.

[0132] In the foregoing and in the examples, all temperatures are set forth uncorrected in degrees Celsius and, all parts and percentages are by weight, unless otherwise indicated.

[0133] The entire disclosures of all applications, patents and publications, cited herein and of corresponding application No. FR 1855789, filed Jun. 27, 2018 are incorporated by reference herein.

IMPLEMENTATION EXAMPLES

[0134] These examples follow the process schemes and the equipment detailed with the aid of the preceding figures.

[0135] Three examples will be described, on five different types of biomass: example 1 on SRC (short-rotation coppice), example 2 on Miscanthus, and example 3 on straw, Example 4 on another straw configuration, and Example 5 on another configuration on SRC.

[0136] The object is to obtain sugary liquors J1 with a minimum sugar concentration of 50 g/kg.

[0137] In the examples described below, the abbreviation DM denotes the dry matter content which is measured according to the standard ASTM E1756-08(2015) Standard Test Method for Determination of Total Solids in Biomass.

[0138] The operating conditions are as follows:

[0139] The mixer M is a Parimix IMR continuous mixer, which allows repulping of marcs with high contents of dry matter (DM) and solids. It is heated by electric means to about 40-50 C.

[0140] Separation on the belt filter F, such as the BFR continuous belt filter from the company BHS with counter-current washing, makes it possible to extract liquors concentrated in sugars. The band filter technology is based on vacuum filtration. The principle is to spread the pretreated marc sequentially over an advancing belt. This porous belt makes it possible, by vacuum suction, to separate the liquids (the liquors) from the solid, forming a cake (the washed marc), which falls at the end of the belt. The liquors are partially recycled.

[0141] The filter F has 10 active vacuum zones, where various steps of the washing and filtration process may take place (movable zones in the filter). The zones are pooled in three groups of zones, which are modulable, and which make it possible to extract three liquors J1, J2 and J3. The filter is equipped, on the sides of the porous belt, with polyurethane or silicone belts, to limit the losses of vacuum observed and to improve the filtration of the product. The filter is equipped with a vertical wall above the belt just after the mixture feed zone to allow better distribution of the mixture on the filter.

[0142] To increase the recovery of the soluble sugars and to reduce the filtration time, the recycled liquor streams J2 (and, where appropriate, J1), J3 and the washing water F1 are heated:

[0143] Liquor J3 is heated and recycled into the first washing water nozzle f1 [0144] The hot washing water was fed via the second washing nozzle f2 [0145] Liquor J2 is heated and recycled up to the repulping of the pretreated marc at the inlet of the mixer (and, where appropriate, the liquor J1).

[0146] For straw (examples 3 and 4), and for example 5 using poplarTCR, a portion of the liquor J1 was also recycled into the mixer M to increase the sugar concentration in the liquor J1.

[0147] The characteristics of the filter and the operating conditions tested are as follows: [0148] Reference: BF025-020, [0149] Gauze: 058000-W120 (Polypropylene 120 m; 05-8000-S120) [0150] Material: polymer [0151] Flow rate: 180 kg/hour of treatable suspension [0152] Filtration surface area: 0.5 m.sup.2 [0153] Vacuum level: between 0.5 and 1 bar

[0154] Table 1 below collates the solids content and dry matter DM content characteristics of the feedstock (pretreated biomass M0) which is separated according to the invention:

TABLE-US-00001 TABLE 1 Example 5: Example 4: Example 3: Example 2: Example 1: SRC (2) Straw (2) Straw Miscanthus SRC Pretreated 44% solid 29-32% solid 29-30% solide 42% solid 38-43% solid Biomass M0 53% MS 41-46% MS 42-44% MS 54% MS 49-53% MS

[0155] The rotation speed of the feed screw of the mixer M, and thus the flow rate of the pretreated marc M0, is defined by the frequency of the metering device D. This speed has an influence on the mixing and the consistency of the repulped marc leaving the mixer. An excessively high mixing screw speed results in a repulped marc that is too viscous for the rest of the process. A weighing hopper is generally provided on the installation (not shown) along with a means for measuring the flow rate of marc, and the feed can be regulated by slaving the screw speed to this flow rate measurement. It may also be chosen to operate with a set screw speed, which will have been calibrated beforehand.

[0156] Table 2 below presents the flow rates of raw marc and of recycled liquor entering the mixer:

TABLE-US-00002 TABLE 2 Flow rate of raw marc recycled liquor inlet (kg/h) (kg/h) SRC (2) (example 5) 50 130 Straw (2) (example 4) 50 130 Straw (example 3) 50 129 Miscanthus (example 2) 70 95 SCR (example 1) 50 75

Example 1 According to the Invention: Biomass Based on Short-Rotation Coppice (SRC)

[0157] The tests began with an SRC, which is often considered as a raw material that is difficult to process. To improve the extraction, spraying nozzles were installed, a vacuum of 0.6 bar was overall material balance and the operating conditions are detailed in table 3 above.

TABLE-US-00003 TABLE 3 Units SRC(2) Straw (2) SRC Straw Miscanthus Flow rate M0 kg/h 50 50 50 50 70 Flow rate recycled J2 kg/h 110 110 75 110 90 Flow rate recycled J1 kg/h 20 20 0 20 0 Flow rate at outlet kg/h 180 180 125 180 160 of the mixer M Feed time s 19 17 19 17 15 Vacuum pressure bar 0.6 0.45 0.6 0.45 0.15 Pressing pressure bar 3.3 3.7 2.6 Temperature J1) C. 40 45 39 45 32 Flow rate kg/h 67 50 45 70 55 Temperature J2 C. 80 80 75 75 75 after exchanger Flow rate J2 kg/h 75 110 75 115 90 produced Temperature J3 C. 80 80 75 75 75 after exchanger Flow rate J3 kg/h 75 105 60 105 80 Flow rate of kg/h 70 69 55 83 55 washing water Temprature C. 50 50 50 50 50 Temperature of washing water Temperature M1 C. 26 35 40 35 45 Flow rate M1 kg/h 60 65 60 52 92

Example 2 According to the Invention: Biomass Based on Miscanthus

[0158] The extraction of the liquor on the pretreated marc obtained from Miscanthus posed no problems. The washing (also referred to as mixing, performed by the mixer M) is very efficient and liquors with a sugar concentration of between 58-60 g/kg were produced. The overall material balance and the operating conditions are detailed in the preceding table, and in table 4 below.

[0159] The belt filter F was fed with 160 kg/h of MoRe (18% DM) at 58 C. Two overflow washing nozzles were installed on zones 4 and 6 of the 10 active zones of the belt. To have the greatest possible space between the streams, the first nozzle washed counter-currentwise relative to the direction of advance of the filter, and the second co-currentwise. 45 kg/h of liquor J1 at 65-68 g/kg of sugars were produced in the first two days. Next, on the third day, the washing water flow rate was increased to produce more liquor with a slightly lower concentration. Consequently, 55 kg/h of J1 were produced with a sugar concentration of between 58 and 60 g/kg.

Example 3 According to the Invention: Biomass Based on Straw

[0160] The first test on straw was performed with the same configuration as for the two preceding examples. Consequently, liquor J1 has a low sugar concentration, of 38.77 g/kg. To increase it, recycling of J1 (20 kg/h) into the J2 tank was established and the mixture of the liquors J1 and J2 was heated and recycled into the mixer M. To improve the vacuum and close the cake which had a tendency to crack, the first washing nozzle was by spraying (zone 4) and the second by overflow (zone 6). Specifically, 70 kg/h of liquor J1 at 53-57 g/kg of sugars were produced. The operating conditions are detailed in the preceding table 4.

Example 4 According to the Invention: Straw Biomass

[0161] This test has the same configuration as in Example 3, also with straw-based biomass, therefore, with the following differences: here the final press (pressing the washed mare cake at zone 9 of the belt filter) is not used, the first washing nozzle is used by pouring and non-spraying, and the second washing nozzle is used by spraying and not pouring, Juice J1 produced has a higher concentration of sugars (50-66 g/kg of sugar). The operating conditions are detailed in Table 4 below.

Example 5 According to the Invention: Biomass Based on SRC

[0162] This test has the same configuration as Example 1, also with a SRC-based biomass, with the following differences: here, the final press (pressing the washed marc cake at zone 9 of the band filter) is not used, and the first wash nozzle is used by pouring and not spraying. The juice J1 produced has a concentration of 51 g/kg of sugar. The operating conditions are detailed in Table 4 below.

[0163] To rapidly check on site if the sugar concentration in liquor J1 indeed reached 50 g/kg as demanded, measurements were taken with an Atago brand PAL-1 refractometer.

[0164] Table 4 below presents the feedstock characteristics: a mixture of M0 with liquors J2 (or J1+J2 for straw) and the products J1 and M0 and quantifies the efficiency of the separation obtained with the invention: the separation of straw was most efficient (99%).

TABLE-US-00004 TABLE 4 Ex 5: Ex 4: Ex 3: Ex 2: Ex 1: SRC (2) Straw(2) Straw Miscanthus SRC Feedstock Pretreated 44% solids 29-32% solids 29-30% solids 42% solids 38-43% solids biomass M0 53% DM 41-46% DM 42-44% DM 54% DM 49-53% DM 80 g/kg 65-93 g/kg ~90 g/kg ~95 g/kg ~83 g/kg of sugar of sugar of sugar of sugar of sugar Recycled ~0% solids ~0% solids ~0.003% solids ~0% solids ~0% solids liquor J2 4% DM 5-11% DM 6% DM 4% DM 8.6% DM 23 g/kg 22-37 g/kg ~33 g/kg ~27 g/kg ~50 g/kg of sugar of sugar of sugar of sugar of sugar Pretreated 12% solids 8.3% solids 8.5% solids 18% solids 16% solids biomass 18% DM 18% DM 16% DM 26% DM 25% DM M0Re Product J1 ~0.04% solids ~0.04% solids ~0.03% solids ~0.09% solids ~0.07% solids 8% DM 10-11% DM 9-10% DM 9-10% DM 11% DM 51 g/kg 50-66 g/kg 53-57 g/kg 5-60 g/kg 69-70 g/kg of sugar of sugar of sugar of sugar of sugar M1 38% solids 23-26% solids 30-32% solids 31-33% solids 33-34% solids 40% DM 28-30% DM 32-33% DM 37-38% DM 35-37% DM 26 g/kg 19-36 g/kg 0.3-1 g/kg 32-38 g/kg 13-20 g/kg of sugar of sugar of sugar of sugar of sugar Separation E ~85% ~71-77% 99% ~62% ~79% efficiency

[0165] In conclusion, it is seen that these five examples according to the invention, with different initial biomasses, managed to achieve the objective of an extracted liquor J1 with the ofsired sugar concentration, largely above the set minimum threshold of 50 g/kg. The separation according to the invention with the two lines of equipment in series, continuous mixer and continuous (belt) filter, allows a lot of flexibility and great compactness. They can thus be inserted without difficulty into a biomass treatment installation at various steps, as soon as there is a need to perform a solid/liquid separation on a mixture with a ofsire to upgraof both the solid part and the liquid part obtained after separation.

[0166] The invention thus makes it possible, irrespective of the pretreated biomass and its rheological constraints, to obtain a sugary liquor with a concentration of greater than 50 g/kg, which is not the case when the invention is not performed, as shown in the following comparative examples:

Comparative Examples (not in Accordance with the Invention)

[0167] The pretreated biomasses of two of the preceding examples are used in a configuration not in accordance with the invention: the substrate M0 is mixed in a mixer M with water and then separated on the belt filter F. In this implementation not in accordance with the invention, there is no recycling of a stream extracted from the belt filter F to the mixer M.

Comparative Example 6: Biomass Based on SRC

[0168] The SRC pretreated biomass M0 ofrived from Example 1 is mixed in a mixer M with water and then separated on the belt filter F, which is itself operated according to the configuration of Example 1. Owing to its rheology, the SRC pretreated biomass must be diluted to a solids content of less than 16% to form a cake that is able to be filtered on the belt filter F. The composition of the SRC marc M0 of Example 1 is recalled: solids content of 38%, sugar content of 83 g/kg. To obtain a correct rheology at the mixer outlet, it is necessary to lower the solids content of the substrate after mixing: it is thus necessary to add 68.8 kg of water to 50 kg of marc M0 into the mixer, and this mixture is then ofposited on the belt filter. The first zone of the belt filter allows the production of a concentrated liquor J1 with a sugar content of only 41.6 g/kg. In this example not in accordance with the invention, it is seen that it is not possible to achieve a concentration of 50 g/kg of sugars in liquor J1 for the SRC substrate.

Comparative Example 7: Biomass Based on Straw

[0169] The straw pretreated biomass M0 ofrived from Example 3 is mixed in a mixer M with water and then separated on the belt filter F, which is itself operated according to the configuration of Example 3. Owing to its rheology, the straw pretreated biomass must be diluted to a solids content of less than 9% to form a cake that is able to be filtered on the belt filter F. The composition of the straw marc M0 of Example 3 is recalled: solids content of 30%, sugar content of 90 g/kg. To obtain a correct rheology at the mixer outlet, it is necessary to lower the solids content of the substrate after mixing: it is thus necessary to add 117 kg of water to 50 kg of marc M0 into the mixer, and this mixture is then ofposited on the belt filter. The first zone of the belt filter allows the production of a concentrated liquor J1 with a sugar content of 27 g/kg. In this example not in accordance with the invention, it is seen that it is not possible to achieve a concentration of 50 g/kg of sugars in liquor J1 for the straw substrate.

[0170] The preceding examples can be repeated with similar success by substituting the generically or specifically described reactants and/or operating conditions of this invention for those used in the preceding examples.

[0171] From the foregoing description, one skilled in the art can easily ascertain the essential characteristics of this invention and, without departing from the spirit and scope thereof, can make various changes and modifications of the invention to adapt it to various usages and conditions.