LIGNOCELLULOSIC BIOMASS TREATMENT METHOD

Abstract

The invention relates to a process for treating a lignocellulosic biomass comprising a solids content of not more than 80% by weight, said process comprising the use of at least one reactor (9,14) for treating said biomass, in which the or at least one of said reactors is fed with biomass via a feed means (6,11) creating a pressure increase between the biomass inlet and the biomass outlet of said feed means, in which said feed means is washed by circulation of a washing fluid between a washing inlet (7,12) and a washing outlet (8,13). According to the process, at least a portion of the washing fluid (8,13) exiting the fluid outlet of the at least one feed means (6,11) is reintroduced into the washing inlet of the same feed means or of another of said feed means.

Claims

1. A process for treating a lignocellulosic biomass comprising a solids content of not more than 90% by weight, said process comprising the use of at least one reactor for treating said biomass (9,14), in which the or at least one of said reactors is fed with biomass via a feeder (6,11) creating a pressure increase between the biomass inlet and the biomass outlet of said feeder, in which said feeder is washed by circulation of a washing fluid between a washing inlet (7,12) and a washing outlet (8,13), characterized in that at least a portion of the washing fluid exiting the fluid outlet of the or of at least one of the feeder (6,11) is reintroduced into the washing inlet of the same feeder or of another of said feeder.

2. The process as claimed in claim 1, characterized in that liquid is extracted from the biomass during its passage through the or one of the feeder (6,11).

3. The process as claimed in claim 1, characterized in that the pressure increase created in the or at least one of the feeder (6,11) is at least 0.05 MPa, notably between 0.05 and 4 MPa.

4. The process as claimed in claim 1, characterized in that it comprises a step of impregnating the biomass with an impregnation liquor containing a chemical catalyst, which is performed by introducing the biomass into the/one of the reactors (9,1) equipped with the feeder (6,11).

5. The process as claimed in claim 1, characterized in that it comprises a step of impregnating the biomass with an impregnation liquor containing a chemical catalyst by passing the biomass through a bed of liquor or by spraying the biomass with the liquor on a conveyor of belt type (9) or by passing the biomass through a stirred reactor.

6. The process as claimed in claim 1, characterized in that it comprises a step of impregnating the biomass with an impregnation liquor containing a chemical catalyst, by introduction into a reactor (9) via said or at least one of said feeder (6).

7. The process as claimed in claim 1, characterized in that it comprises a step of treating the biomass by cooking, notably in the or one of the reactors (14) equipped with a feeder (11).

8. The process as claimed in claim 1, said process comprising the following steps: a) a Preparing an impregnation liquor (4) containing a chemical catalyst (2) intended for the impregnation of the biomass (5), chosen from an acid catalyst, a basic catalyst and an oxidizing catalyst, and preferably an acid catalyst, in a preparation zone (3) b) Introducing the milled biomass (5) via an inlet of an impregnation reactor (9) by a first feeder (6), said first feeder being washed by circulation of a first washing fluid (7,8) between an inlet and an outlet of said first feeder (6) c) Introducing the liquor into the impregnation reactor (9) via a first liquor (4) inlet of the reactor d) Transferring the impregnated and drained biomass (10) from an impregnation reactor outlet to an inlet of a cooking pretreatment reactor (14), the introduction into said pretreatment reactor taking place via a second feeder (11), said second feeder being washed by circulation of a second washing fluid (12,13) between an inlet and an outlet of said second feeder e) Pretreating said biomass (10) in said steam explosion reactor (14) f) Reintroducing at least a portion of the first and/or of the second washing fluid leaving the fluid outlet of said first or of said second feeder (6,11) into the washing inlet of the first feeder (6) and/or of the second feeder (11).

9. The process as claimed in claim 1, characterized in that it also comprises: g) Reintroducing a portion of the first and/or of the second washing fluid leaving the fluid outlet of the first or of the second feeder (6,11) into the impregnation liquor preparation zone (3) for the purpose of preparing a) said liquor.

10. The process as claimed in claim 1, characterized in that the and/or at least one of the feeder is a feed screw (6,11), which is notably at least partly conical, comprising a cowling equipped with a grate allowing the circulation of the washing fluid and optionally the extraction of fluid from the biomass.

11. The process as claimed in claim 7, characterized in that a portion of the first washing fluid (8) at the washing outlet of the first feeder (6) is reintroduced into the washing inlet (8b,8d) of the first or of the second feeder, and in that another portion of said washing fluid is reintroduced (8c) into the liquor preparation zone (3) for the purpose of preparing same.

12. The process as claimed in claim 7, characterized in that a portion of the second washing fluid (13) at the washing outlet of the second feeder (11) is reintroduced (13b,13d) into the washing inlet of the first or of the second feeder (6,11), and in that another portion (13c) of said washing fluid is reintroduced into the liquor preparation zone (3) for the purpose of preparing same.

13. The process as claimed in claim 1, characterized in that the washing of the feeder (11) is performed in the presence of biomass supplemented with a catalyst, notably an acid, basic or oxidizing catalyst, in that the washing fluid leaving the fluid outlet of said feeder (6,11) contains a certain content of said catalyst when the biomass undergoes a liquid extraction by passing through said feeder, and in that said washing fluid containing this catalyst is at least partly reintroduced into the washing inlet of the same feeder or of another of said feeder, notably conveying biomass free of catalyst.

14. A facility performing the process as claimed in claim 1, characterized in that it comprises at least one reactor for treating a lignocellulosic biomass having a solids content of not more than 90% by weight with feeding of the or of at least one of said reactors with biomass via a feeder creating a pressure increase between the biomass inlet and the biomass outlet of said feeder, with washing of said feed feeder by circulation of a washing fluid between a washing inlet and a washing outlet, and a line for reintroducing at least a portion of the washing fluid (8,13) exiting the fluid outlet of the or of at least one of the feeder (6,11) into the washing inlet of the same feeder or of another of said feeder.

15. A facility for treating a lignocellulosic biomass, comprising: A zone (3) for preparing an impregnation liquor (4) containing a chemical catalyst for the impregnation of the biomass (5), chosen from an acid, basic or oxidizing catalyst, and preferably an acid catalyst, and equipped with a liquor outlet An impregnation reactor (9), said reactor being equipped with a biomass inlet and outlet A first feeder (6) for feeding milled biomass to the impregnation reactor (9) via the biomass inlet of the impregnation reactor A feeder for feeding impregnation liquor (4a) to the reactor (5) connecting a liquor outlet of the liquor (4) preparation zone (3) to a first liquor inlet in the impregnation reactor A reactor (14) for pretreatment of the impregnated biomass (10) by cooking, a biomass inlet of which is connected to the biomass outlet of the impregnation reactor (9) A second feeder (11) for feeding impregnated biomass (10) to the pretreatment reactor via the biomass inlet of said pretreatment reactor (14) A circulation of washing fluid (7,8) between an inlet and an outlet of the first milled biomass (5) feeder (6) of the impregnation reactor (9) A circulation of washing fluid (12,13) between an inlet and an outlet of the second impregnated biomass (10) feeder (11) of the pretreatment reactor (14) characterized in that the facility also comprises A line for reintroducing at least a portion of the first and/or of the second washing fluid leaving the fluid outlet of said first or of said second feeder (6,11) into the washing inlet of the first feeder and/or of the second feeder.

16. The process as claimed in claim 1, wherein the lignocellulosic biomass (5) is wood, straw, agricultural residues, or dedicated energy crops, notably annual or perennial plants such as miscanthus.

17. The process as claimed in claim 1, which produces sugars, biofuels or biobased molecules.

18. The process as claimed in claim 1, wherein the feeder (6,11) is a feed screw, which is at least partly conical, and comprises a cowling equipped with a grate allowing the circulation of washing fluid.

Description

DETAILED DESCRIPTION

[0079] The invention will be described in detail below with the aid of nonlimiting examples of the process according to the invention, illustrated by the following figures:

[0080] FIG. 1: a synoptic representation, of block diagram type, of the general principle of the biomass treatment process according to the invention,

[0081] FIG. 2: a synoptic representation, of block diagram type, of a first embodiment of the biomass treatment process according to the invention,

[0082] FIG. 3: a synoptic representation, of block diagram type, of a second embodiment of the biomass treatment process according to the invention,

[0083] FIG. 4: a synoptic representation, of block diagram type, of a third embodiment of the biomass treatment process according to the invention.

[0084] FIG. 1 is thus the representation of the principle of the invention, FIG. 2 concentrates on two biomass treatment steps: catalytic impregnation and then cooking. FIGS. 3 and 4 describe the whole process for treating biomass up to its enzymatic hydrolysis, after impregnation and cooking.

[0085] The invention is more particularly focused on the first two steps, namely impregnation of the milled biomass and treatment by cooking of the biomass once it has been impregnated.

DESCRIPTION OF THE FIGURES USING THE FOLLOWING REFERENCES

[0086] The same references correspond to the same components/fluids/products on all of the figures: [0087] 1: Entry of water into the liquor preparation tank [0088] 2: Entry of acid into the liquor preparation tank [0089] 3: Liquor preparation tool (tank) [0090] 4: Acidic liquor to the impregnation tool (reactor) [0091] 5: Milled biomass [0092] 6: Screw or plug-screw feeder of the impregnation tool [0093] 7: Water for washing the plug-screw feeder of the impregnation tool [0094] 8: Washing liquid outlet of the plug-screw feeder of the impregnation tool [0095] 9, 9: Impregnation tool (reactor) [0096] 9a: Impregnation zone of the impregnation tank 9 [0097] 9b: Draining zone of the impregnation tank 9 [0098] 10: Impregnated and drained biomass [0099] 11: Screw or plug-screw feeder of the pretreatment tool [0100] 12: Water for washing the plug-screw feeder of the pretreatment tool [0101] 13: Press liquor of the plug-screw feeder of the pretreatment tool [0102] 13.a: Press liquor to the purge [0103] 13.b: Recycling of the press liquor for washing the plug-screw feeder of the pretreatment tool [0104] 13.c: Recycling of the press liquor into the acidic liquor preparation tank 3 [0105] 13.d: Recycling of the press liquor for washing the plug-screw feeder of the impregnation tool [0106] 14: Pretreatment cooking tool (explosion reactor) [0107] 15: Injection of steam for the pretreatment [0108] 16: Pretreated biomass and steam [0109] 17: Tool (cyclone) for separating steam and pretreated biomass [0110] 18: Steam to condensation [0111] 19: Pretreated biomass [0112] 20: Enzymatic hydrolysis [0113] 21: Enzymatic hydrolysis must containing sugars [0114] 22: Alcoholic (ethanolic) fermentation [0115] 23: Fermentation wine containing ethanol (alcohol) [0116] 24: Distillation [0117] 25: Concentrated alcohol [0118] 26: Crude vinasses

[0119] FIG. 1 very schematically represents the principle of the invention in its simplest embodiment (process of which the details and various steps will be subsequently described with the aid of FIGS. 2 to 4): the biomass 5,10 (impregnated or not impregnated with a catalytic liquor) is introduced into a reactor 9,14 for a treatment, by a pressurized feed means 6,11 which is a screw (also known as a plug screw feeder) whose end portion is conical, which has a cowling with a draining grate, a washing water inlet 7,12 and a washing water outlet 8,13. A hermetic biomass plug becomes created in the downstream portion of the screw, which creates a compression on the biomass reflected by a pressure difference between the biomass inlet and the biomass outlet of the screw of at least 0.05 MPa, for example about 0.5 MPa. The compression applied to the biomass may lead to the expulsion of a portion of the liquid contained in the biomass, notably when the SC of the biomass is less than 80% before it enters the pressurized feed means 6,11. The liquid thus extracted becomes mixed with the washing water and is withdrawn with the spent washing water 8,13.

[0120] According to the invention, at least a portion of the washing water leaving the screw 8,13 is reinjected into the washing water inlet 7,12 of the screw. It is noted that it remains possible for a portion of the exiting washing water to be simply purged, and for a portion of the entering washing water to originate from a water supply as in the prior art, to supplement the amount of water recycled into the screw inlet, periodically or systematically.

[0121] In this representation, the recycling of the washing water applies to the same screw, but, as will be detailed with the other figures, the invention also relates to the total or partial recycling of the washing water at the outlet of one screw into the inlet of another feed screw, when the process envisages several feed screws for several reactors.

[0122] The solids content of the biomass entering the feed screw is, here, 50%. It may occur that a portion of the liquid of the biomass is extracted during its transportation in the screw, this extracted water becoming mixed with the spent washing water at the washing outlet of the screw. The lower the solids content of the biomass, the more extraction of fluid there will be from the biomass in the feed screw, this fluid supplementing or even optionally totally replacing the washing fluid at the screw inlet.

[0123] FIG. 2 represents a step of impregnation of the biomass with an acidic liquor, followed by a cooking step forming part of a biomass treatment:

[0124] The process proceeds in the following manner: The water and the acid are introduced, respectively, via pipes 1 and 2 into the acidic liquor preparation tank 3. The acidic liquor of pipe 4 is then injected into an impregnation device 9 to be mixed with the milled biomass. The impregnation device is, here, a conveyor, of the conveyor belt type driven in translation by rotation of rollers supporting the belt, on which belt is placed the biomass to a given thickness. While it is being conveyed, the biomass is subjected to spraying with acidic liquor taken from the tank 3, via nozzles placed above the belt. The excess liquor may be recovered under the belt in a collection zone, to be optionally totally or partly recycled.

[0125] The impregnated biomass 10, which has optionally been drained beforehand, is introduced into the treatment unit 14 by means of another feed screw of plug screw feeder type 11 which compresses the biomass to form a biomass plug. This hermetic biomass plug ensures the leaktightness and prevents leakages of steam, when the cooking reaction in this biomass reactor 14 takes place by steam explosion. During this compression in the screw 11, a solid/liquid separation takes place, and the spent acidic liquor is evacuated through the cowling grate of the screw. This screw is washed with water from pipe 12 which thus becomes mixed with spent acidic liquor, and the mixture of washing water and of spent acidic liquor (known as press liquor) is evacuated in pipe 13. The press liquor may also contain solid derived from the washing of the screw 11.

[0126] Optionally, a solid/liquid separation step is performed on this stream 13, for example with a device using a grate of curved shape.

[0127] The stream 13 can then be directed toward: [0128] a purge via pipe 13a [0129] recycling via pipe 13b to replace all or some of the water 12 for washing the screw 11 [0130] recycling into the acidic liquor preparation tank 3 via pipe 13c.

[0131] Various possibilities then become available: [0132] according to one embodiment, all of the stream 13 is sent into pipe 13b to replace all or some of the washing water 12, [0133] according to another embodiment, only a part of the stream 13 is sent into pipe 13b to replace all or some of the washing water 12, and the rest is sent via pipe 13c to contribute toward the manufacturing of liquor (for example in a volume proportion between the two variants of between 20/80 and 80/20).

[0134] The biomass is treated in the treatment tool 14 by cooking and steam explosion in the manner described in the following figures. FIG. 3 presents a variant relative to FIG. 2 in the way of performing the impregnation of the biomass, and it also represents the steps subsequent to the cooking/steam explosion of the biomass.

[0135] Only the differences with the process according to FIG. 2 will be described here, the two processes being otherwise performed identically.

[0136] The water and the acid are introduced, respectively, via pipes 1 and 2 into the acidic liquor preparation tank 3. The acidic liquor of pipe 4 is then injected into an impregnation device 9 to be mixed with the milled biomass. It is, here, a reactor, which is positioned substantially vertically here.

[0137] The premilled biomass is introduced into the process via pipe 5 in a feed screw 6, similar to the screw 11 already described in the preceding figure, also with a water washing circuit. This screw makes it possible to form a hermetic biomass plug which ensures the leaktightness and prevents leakages of acidic liquor. This screw is washed with water which enters via pipe 7 and leaves via pipe 8. At the screw outlet, expansion of the plug takes place in the bottom zone of the impregnation reactor 9. The biomass becomes impregnated with acidic liquor in the impregnation zone 9a before being drained in the draining zone 9b. It is conveyed into the reactor 9 via one or two transportation screws.

[0138] The stream 13 can then be directed, as previously, toward: [0139] a purge via pipe 13a [0140] recycling via pipe 13b to replace all or some of the water 12 for washing the screw 11 [0141] recycling into the acidic liquor preparation tank 3 via pipe 13c; [0142] but another possibility also becomes available, since, here, the stream 13 can also be recycled via pipe 13d to replace all or some of the water 7 for washing the screw 6.

[0143] Continuing with the more detailed description of the reactor 14 common to FIGS. 2 to 4 and to the steps following the treatment in this reactor 14:

[0144] The steam required for heating the reactor 14 is introduced via pipe 15. At the reactor outlet, the biomass/steam mixture is expanded and conveyed via line 16 to the separation tool 17. The separation tool 17 may be of cyclone type: it allows the separation of the steam 18 from the pretreated biomass 19.

[0145] The pretreated biomass is then transformed in the transformation tool 20 into a must 21 containing sugars, using an enzymatic cocktail. The sugars are converted into alcohol (e.g. ethanol, acetone, butanol) by fermentation in the fermentation step 22. The fermentation wine 23 is sent to a separation and purification step 24. Step 24, which is performed, for example, by distillation, allows the separation of a stream 25 containing the concentrated alcohol from the crude vinasses (spent water, residual lignin) 26.

[0146] The details of the operating conditions for the steam explosion, must conversion and fermentation steps, which are considered as being known to those skilled in the art, will not be given here.

[0147] FIG. 4 shows a variant relative to FIG. 3.

[0148] The additional references relative to FIG. 3 are: [0149] 8: Spent washing liquid outlet of the impregnation tool screw 6 [0150] 8.a: Spent washing liquid to the purge [0151] 8.b: Recycled washing liquid for washing the impregnation tool screw [0152] 8.c: Washing liquid recycled into the acidic liquor preparation tank 3 [0153] 8.d: Recycled washing liquid for washing the screw 11 of the pretreatment tool 14

[0154] Only the differences with the process according to FIG. 3 will be described here, the two processes being otherwise performed identically:

[0155] Here, the water 8 for washing the feed screw 6 is also recycled according to various alternative or cumulative possibilities. The liquid 8 for washing the transfer screw 6 may be either: [0156] purged from the system via pipe 8a [0157] recycled via pipe 8b to replace the water 7 for washing the feed screw 6 of the impregnation reactor 9 recycled via pipe 8c into the acidic liquor tank 3 [0158] recycled via pipe 8d to replace the water 12 for washing the feed screw 11 of the explosion tool/reactor 14.

[0159] According to another embodiment of the invention, all of the stream 8 is sent into pipe 8b or into pipe 8d to replace all or some of the washing water 12 or 7. According to another embodiment, a portion is sent into pipe 8b or 8b, and the rest is sent via pipe 8c to contribute toward the preparation of the impregnation liquor. The ratio between the two parts, by volume, may be between 80/20 and 20/80.

[0160] In any case, as thus regards the recycling either of the spent water from the screw 6 or of the press liquor from the screw 11, a portion may also be taken to be sent to the purge (pipes 13a, 8a).

[0161] Needless to say, it is also within the context of the invention to combine the recycling of the spent water from the washing of the screw 6 with that of the press liquor from the screw 11, or to recycle only one or the other.

[0162] A few operating details or variants are given below for the first two biomass treatment steps described previously:

[0163] The impregnation step is performed at a temperature ranging from 10 to 95 C., and the residence time of the biomass in said impregnation step is between 20 seconds and 12 hours. Preferably, the residence time of the biomass is between 30 seconds and 60 minutes.

[0164] The impregnation step may be performed in batch or continuous mode. Preferably, this step is performed in continuous mode. The impregnation step is preferably performed at atmospheric pressure. Preferably, the impregnation step is performed in a single step.

[0165] The impregnation step involves placing in contact the biomass and the acidic liquor. It may be performed, for example, by dipping or by spraying.

[0166] The impregnation step is performed in equipment known to those skilled in the art, for example in a stirred reactor, by horizontal or vertical throughput of the biomass in a bed of liquor, by spraying on a belt transporting the biomass (as seen in FIG. 2) or in a transportation screw.

[0167] The impregnation reactor or impregnator is generally equipped with one or more tools which transfer(s) the lignocellulosic substrate from its entry to the outlet aperture. These tools may be, for example, screws or belts. The impregnator is moreover equipped with one or more pipes for conveying the acidic liquor and also, if need be, one or more pipes for withdrawing acidic liquor. Said acidic liquor inlet and outlet pipes are generally installed so as to function by cocurrent or counter-current recycling.

[0168] The Pretreatment Step (Cooking):

[0169] The lignocellulosic substrate undergoes this pretreatment step, which is notably directed toward modifying the physical and physicochemical properties of the cellulosic fraction, such as its degree of polymerization and its state of crystallinity.

[0170] The pretreatment includes a cooking zone. This cooking is performed at a temperature of between 100 C. and 250 C., and more preferentially between 130 C. and 230 C., at a pressure of between 0.1 and 4 MPa. The residence time in the cooking zone is between 10 seconds and 4 hours, and more preferentially between 3 minutes and 1 hour.

[0171] The cooking may take place in batch or continuous mode. It may be performed in any equipment known to those skilled in the art, for example a stirred reactor, a horizontal tubular reactor equipped with a transportation screw, a non-stirred batch reactor, etc. The thermal energy required for the cooking may be supplied via a heat exchange with a heat-transfer fluid (indirect), by electrical heating, or by direct injection of a hot fluid, for example pressurized water or steam.

[0172] The exit of the solid at the end of cooking may take place by rapid decompression, by slow decompression, after a temperature reduction induced by direct or indirect heat exchange, etc.

[0173] In one embodiment (preferred), the cooking zone is heated with steam by direct injection and is followed by abrupt decompression of the medium, this process being known as steam explosion (or steamex). This is a process in which the lignocellulosic substrate is rapidly brought to a high temperature by injecting pressurized steam. Stoppage of the treatment takes place by abrupt decompression.

[0174] The operating conditions of the steam explosion process are as follows: [0175] steam is injected directly into the reactor; [0176] the temperature of the reactor is generally between 150 and 250 C., preferably between 160 C. and 220 C., [0177] the pressure is between 0.5 and 2.5 MPa, more preferentially between 0.8 and 2.0 MPa, [0178] the residence time before the expansion phase ranges from 10 seconds to 25 minutes, and preferably between 3 minutes and 15 minutes.

[0179] The steam explosion may be performed in batch or continuous mode and the depressurization step which permits destructuring of the biomass may proceed in one or more steps.

[0180] Examples of implementation of this or these recycling operations using the process according to FIG. 4 are now described:

Comparative Example 1

[0181] This is an example with recycling of only the spent washing waters as top-up water for the liquor preparation tank. The biomass to be treated is wood having the following features:

[0182] Feedstock: Poplar wood, flow rate 7.47 tons/hour, solids content (SC): 50%, mean composition (SC basis):

TABLE-US-00001 % (SC basis) Cellulose 42.6% Hemicellulose 20.5% Lignin and others (ash, extractable matter, etc.) 36.9%

[0183] The acronym SC denotes the solids content, which is measured according to the standard ASTM E1756-08(2015) Standard Test Method for Determination of Total Solids in Biomass.

[0184] The wood is used in the form of chips with a characteristic size of 50 mm. The temperature of the chips entering the unit is room temperature. The chips 5 are conveyed to the impregnation reactor 9 via the conical screw 6. This screw is washed with washing water 7,8 at a flow rate of 1 ton/hour. During the compression performed by the screw 6, liquid is extracted from the poplar chips at a rate of 0.679 ton/hour, the total flow rate of spent water for washing the screw 6 of the impregnation reactor 9 is thus 1.679 tons/hour.

[0185] The following are introduced into the impregnation reactor 9: [0186] the compressed wood chips, via the conical screw 6 [0187] 2.9 tons/hour of an acidic liquor 4 prepared with water 1 and sulfuric acid 2 at a mass concentration of 1.57% by weight (wt), at a temperature of 90 C.

[0188] The impregnated chips are removed from the impregnation reactor 9 and transferred to a steam explosion reactor 14. Entry into the pretreatment reactor takes place by transfer by means of another conical screw 11. This screw is washed with washing water at a flow rate of 0.6 ton/hour. During the compression performed by the screw 11, liquid is extracted from the impregnated poplar chips at a rate of 2.95 tons/hour, the total flow rate of spent water for washing the screw 6 of the impregnation reactor 9 is thus 3.55 tons/hour. This stream contains 0.5% by weight of H.sub.2SO.sub.4.

[0189] The steam explosion pretreatment is performed at 200 C. in a continuous configuration using a short residence time. The medium is abruptly expanded to a pressure of 1.3 atm.

[0190] The acidic liquor preparation tank 3 located upstream of the impregnation delivers a flow rate of 2.9 tons/hour of acidic liquor. This liquor is prepared with water and 96% sulfuric acid, the respective flow rates are 2.8526 tons/hour of water and 0.0474 ton/hour of acid at a concentration of 96% by weight. The total consumption of water in this configuration is 4.5526 tons/hour and the total consumption of acid is 0.0474 ton/hour of sulfuric acid at a concentration of 96% by weight.

[0191] The spent waters from the washing of the screws 6 and 11 are sent to the purge via pipes 8a and 13a.

Comparative Example 2

[0192] This repeats comparative example 1, the only difference here being that a portion 13c of the stream obtained from the washing of the screw 11 of the explosion reactor 14 is sent to the acidic liquor preparation tank 3: this flow is equal to the liquid top-up required taking into account the top-up of acid that should be made to have the target acidity. Thus, the flow rate of recycled liquid is 2.8675 tons/hour and the flow rate of top-up acid is 0.0325 ton/hour of sulfuric acid at 96% by weight. In this second configuration, the total consumption of water is 1.6 tons/hour (for the washing of the screw 11) and the consumption of acid is 0.0325 ton/hour of sulfuric acid at 96% by weight. A stream of 2.362 tons/hour of spent waters must be treated.

Example 3 According to the Invention

[0193] In this example, a process of impregnation according to the invention and of pretreatment of wood, treating the same feedstock as in the preceding comparative examples 1 and 2, is presented. The wood is used in the form of chips with a characteristic size of 50 mm. The temperature of the chips entering the unit is room temperature.

[0194] The chips are conveyed to the impregnation reactor 9 via the conical screw 6. This screw is washed with a washing liquid 7,8,13d at a flow rate of 1.0 ton/hour; this liquid originates from the mixture of water 7 and of the liquid 13d for washing the screw 11 of the pretreatment reactor 14. During the compression performed by the screw 6, liquid is extracted from the poplar chips at a rate of 0.679 ton/hour, the total flow rate of spent water for washing the screw 6 of the impregnation reactor 9 is thus 1.679 tons/hour.

[0195] The following are introduced into the impregnation reactor 9: [0196] the compressed wood chips, via the conical screw 6 [0197] 2.9 tons/hour of an acidic liquor 4 prepared with water 1 and sulfuric acid 2 at a mass concentration of 1.57% by weight, at a temperature of 90 C.

[0198] The impregnated chips are removed from the impregnation reactor 9 and transferred to a steam explosion reactor 14. Entry into the pretreatment reactor 14 takes place by transfer by means of a second conical screw 11. This screw 11 is washed with washing water 12,13 at a flow rate of 0.6 ton/hour. During the compression performed by the screw 11, liquid is extracted from the impregnated poplar chips at a rate of 2.95 tons/hour, the total flow rate of spent water for washing the screw 11 of the reactor 14 is thus 3.55 tons/hour. This stream contains 0.5% by weight of H.sub.2SO.sub.4. The steam explosion pretreatment is performed at 200 C. in a continuous configuration using a short residence time. The medium is abruptly expanded to a pressure of 1.3 atm.

[0199] The acidic liquor preparation tank 3 located upstream of the impregnation delivers a flow rate of 2.9 tons/hour of acidic liquor. Preferably, it is equipped with sensors for measuring the pH and the flow rate for the water, acid, spent liquor and prepared liquor.

[0200] A portion of the stream obtained from the washing of the screw 11 of the explosion reactor 14 is sent to the acidic liquor preparation tank 3: this flow is equal to the liquid top-up required, taking into account the top-up of acid that should be made to have the target acidity. Thus, as in the preceding examples, the flow rate of recycled liquid is 2.8675 tons/hour and the flow rate of top-up acid is 0.0325 ton/hour of sulfuric acid at 96% by weight. The part 13d of the stream of spent liquid 13 for washing the screw 11 of the pretreatment reactor 14 which is not sent as top-up liquid for the liquor tank 3 is sent to wash the screw 6 of the impregnation reactor 9, at a flow rate of 0.683 ton/hour, as a supplement to 0.317 ton/hour of water. The total water consumption is thus 0.917 ton/hour. A stream of 1.679 tons/hour of spent waters must be treated.

[0201] Thus, the process according to the invention allows, relative to the configuration of comparative example 2: [0202] a reduction of the mass consumption of water of more than 42% [0203] a 29% reduction in the mass of spent waters to be treated.

Example 4 According to the Invention

[0204] In this example, a process of impregnation according to the invention and of pretreatment of wood, treating the same feedstock as in comparative example 1, is presented.

[0205] The wood is used in the form of chips with a characteristic size of 50 mm. The temperature of the chips entering the unit is room temperature.

[0206] The chips are conveyed to the impregnation reactor 9 via the conical screw 6. This screw is washed with washing water 7 at a flow rate of 1.0 ton/hour. During the compression performed by the screw, liquid is extracted from the poplar chips at a rate of 0.679 ton/hour, the total flow rate of spent water for washing the screw 6 of the impregnation reactor 9 is thus 1.679 tons/hour.

[0207] The following are introduced into the impregnation reactor 9: [0208] the compressed wood chips, via the conical screw 2 [0209] 2.9 tons/hour of an acidic liquor 4 prepared with water 1 and sulfuric acid 2 at a mass concentration of 1.57% by weight, at a temperature of 90 C.

[0210] The impregnated chips are removed from the impregnation reactor 9 and transferred to a steam explosion reactor 14. Entry into the pretreatment reactor 14 takes place by transfer by means of a second conical screw 11. During the compression performed by the screw, liquid 13 is extracted from the impregnated poplar chips at a rate of 2.95 tons/hour. A portion 13b of this stream, 1.5 tons/hour, is used to wash the conical screw 11, according to the invention. The total flow rate of spent water for washing the screw 6 of the impregnation reactor 9 is thus 4.45 tons/hour, of which 1.5 tons/hour are recycled for the washing 13b. This stream contains 0.602% by weight of H.sub.2SO.sub.4. This stream is more concentrated in acid than the stream extracted from example 1, since the spent acidic liquor extracted during the compression has not been diluted with the screw washing water. The steam explosion pretreatment is performed at 200 C. in a continuous configuration using a short residence time. The medium is abruptly expanded to a pressure of 1.3 atm.

[0211] The acidic liquor preparation tank 3 located upstream of the impregnation delivers a flow rate of 2.9 tons/hour of acidic liquor.

[0212] The stream 13 obtained from the washing of the screw 11 of the pretreatment reactor 14 which is not used for the washing 13b of the screw is sent 13c to the acidic liquor preparation tank 3 at a flow rate of 2.87 tons/hour, and the remainder 13a (0.08 ton/hour) is purged. The flow rate of top-up acid is 0.0294 ton/hour of sulfuric acid at 96% by weight.

[0213] In the process according to this example, the total consumption of water is 1.0 ton/hour (for the washing of the impregnation screw 6) and the consumption of acid is 0.0294 ton/hour of sulfuric acid at 96% by weight. A stream of 1.759 tons/hour of spent waters must be treated.

[0214] Thus, the process according to this example in accordance with the invention allows, relative to the configuration of comparative example 2: [0215] a reduction of the mass consumption of water of 37% [0216] a 9.4% reduction in the mass consumption of concentrated sulfuric acid [0217] a 25% reduction in the mass of spent waters to be treated.

[0218] In conclusion, these examples demonstrate that the invention allows very significant energy/starting material savings, with great implementation flexibility. In addition, the modification induced on the facility remains modest and easy to implement, with the addition of pipes equipped, where appropriate, with means for varying the flow rate, for measuring the pH or the temperatures, these additional pipes remaining in their conception entirely within the scope of a person skilled in the art. The invention remains beneficial even if the various operations for treating the biomass (for example the impregnation and cooking and/or steam explosion operation) are not continuous: preference will be given in this case to the recycling of the washing waters to the same feed screw (loop 8b for the washing of the screw 6, loop 13b for the washing of the screw 11).