EP0432015B1 - Verfahren und Einrichtung zur Herstellung einer zumindest 80% Xylose enthaltende Zuckermischung aus einem lignocellulosischen Substrat - Google Patents

Verfahren und Einrichtung zur Herstellung einer zumindest 80% Xylose enthaltende Zuckermischung aus einem lignocellulosischen Substrat Download PDF

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EP0432015B1
EP0432015B1 EP90403374A EP90403374A EP0432015B1 EP 0432015 B1 EP0432015 B1 EP 0432015B1 EP 90403374 A EP90403374 A EP 90403374A EP 90403374 A EP90403374 A EP 90403374A EP 0432015 B1 EP0432015 B1 EP 0432015B1
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Prior art keywords
substrate
impregnation
hydrolysis
reactor
xylose
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French (fr)
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EP0432015A1 (de
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Daniel Ballerini
Francis Nativel
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00—Sugars not otherwise provided for in this class
    • C13K13/002—Xylose

Definitions

  • the invention relates to a method and a unit for the continuous production of a mixture of sugars containing at least 80% by weight of xylose from a lignocellulosic substrate. It applies in particular to the transformation of xylose into xylitol which is a natural sweetener.
  • lignocellulosic substrates wood, annual plants
  • a heterogeneous composition in which there are usually three predominant fractions which are cellulose, hemicelluloses and lignin. This heterogeneity complicates their valuation.
  • a separation of hemicelluloses which have a variable sugar composition but are often rich in pentoses, in particular xylose
  • cellulose composed exclusively of glucose
  • This interest requires that the objective targeted is chemical use or fermentation since if most fermentations use glucose from the hydrolysis of cellulose, fewer are those that use, for example, the pentoses of hemicelluloses.
  • a so-called water vapor explosion treatment is already known in which the lignocellulosic substrate is subjected for a variable time to the action of water vapor under pressure at a temperature generally above 150 ° C. for example 150 at 250 ° C. This action ends with an explosive trigger.
  • This treatment formerly known for improving the digestibility of forages, also increases the susceptibility of lignocellulosic substrates to enzymatic hydrolysis (K. BUCHHOLZ, J. PULS, B. GADELMANN, MM DIETRICHS, Process Biochemistry, Dec / Jan. 1980 / 1981, pp 37-43).
  • This device cannot be used in an acid medium and at high temperature, of the order of 200 ° C., because of the corrosion levels that the hydrolysis treatment in the presence of acid would generate.
  • One of the objects of the invention is to respond to the problems raised above.
  • the device can operate continuously under severe temperature and pressure conditions, for example at a pressure which may be between 1 and 7 bar.
  • the invention is defined by the claims.
  • the invention therefore relates to a process for the continuous production of a mixture of sugars in solution containing at least 80% by weight of xylose from a lignocellulosic substrate comprising a grinding step, an impregnation step in aqueous solution of preferably acid, a hydrolysis step in the presence of water vapor, a dilution step in the presence of water, a step of extracting the mixture of sugars produced from the hydrolyzed substrate, and a step of recovering xylose.
  • the lignocellulosic substrate is generally wood, cobs and stalks of corn or straw. However, we prefer to use corn cobs.
  • the wood is usually debarked and cut in the form of chips while the stems are crushed and obtained at a particle size generally between 0.1 and 40 mm, preferably between 1 and 5 mm.
  • the straw is chopped and used in the form of strands.
  • the term grinding is used for the step of dividing to the appropriate size of each of these substrates.
  • the dry matter content of the substrate is generally at least 50%, for example that of wood is approximately 50% while that of straw is approximately 80% and that of stalks approximately 80%.
  • the impregnation is generally carried out in an impregnation zone, supplied separately or not, with water and an acid. It could be a base if you wanted to do an alkaline treatment.
  • the water and acid supply rate is adjusted as a function of the supply rate of ground substrate, its initial dry matter content, its desired final content and its transfer speed in the impregnation zone.
  • These water and acid flows are advantageously distributed annularly by suitable injection means known to those skilled in the art and generally located in the first quarter of this zone, upstream side.
  • the proportion of acid used relative to the dry matter content of the substrate is generally between 0.1 and 10%, advantageously between 2 and 5%.
  • the dry matter content at the outlet of the impregnation zone is approximately 35 to 55%.
  • the impregnation is generally carried out at ambient temperature and pressure during a residence time which depends on the nature of the substrate used and which is conditioned by the speed of transfer into the impregnation zone and by the percentage of material. dries when entering and leaving this area. It is usually 1 to 60 mins and preferably from 10 to 40 minutes. Operating substantially in the absence of a separate liquid phase, the quantities of reactants and the size of the reactors are minimized.
  • the supply of substrate impregnated with the hydrolysis zone is generally carried out by an airlock controlled by servo and control means connected to a high level measurement in the airlock and to a timer controlling the opening or closing of the airlock valves.
  • This supply is advantageously gravitational and the pressure is balanced by three-way valves connecting the airlock, either to the hydrolysis reactor described below and operating under pressure, or for example to the impregnation reactor operating substantially at pressure. atmospheric.
  • the hydrolysis of the acidified substrate is generally carried out in the presence of medium-pressure water vapor, preferably 1 to 7 bar, advantageously 2 to 5 bar, and at a temperature of 120 to 170 ° C, advantageously of 120 to 150 ° C and preferably from 135 to 145 ° C.
  • the residence time of the substrate in the hydrolysis zone is conditioned by the rate of transfer of the substrate in this zone. It is generally 10 minutes to 1 hour, preferably 20 to 40 minutes. It is all the better controlled as the hydrolysis is carried out in the absence of a separate liquid phase in the hydrolysis reactor.
  • the quantity of vapor introduced is a function of the dry matter content of the acidified substrate and of the operating conditions in temperature and pressure of the hydrolysis reactor. It is introduced with a flow rate such that at the outlet of the hydrolysis zone, the impregnated and hydrolysed substrate contains substantially no separate liquid phase.
  • the dry matter content is then generally between 25 and 55% by weight and preferably from 40 to 50% by weight.
  • the invention also relates to a unit for the continuous production, in particular of xylose, from lignocellulosic substrate.
  • This unit includes means for grinding this substrate to an adequate size connected to means for supplying ground substrate.
  • the unit comprises in combination a reactor for impregnating this ground substrate, of cylindrical shape having an inlet connected to the substrate supply means and an outlet, means for continuously transferring the substrate into the reactor impregnation and means for supplying a solution comprising water and at least one acid (or at least one base), said impregnation reactor comprising control means connected to the substrate supply means, to the means for transferring this substrate into the impregnation reactor and to the means for supplying said solution and adapted to impregnate the substrate under conditions such that it is devoid of a separate liquid phase,
  • the production unit being in further characterized in that it comprises a continuous and pressurized hydrolysis reactor, of cylindrical shape, made of stainless steel comprising at one of its ends a sealed feed member continuous ion of impregnated substrate
  • the transfer means of the impregnation reactor can comprise either a single endless screw for conveying the stalks or a twin screw for the other substrates which are by nature less porous.
  • the hydrolysis reactor can be substantially horizontal or substantially inclined and the member for feeding the impregnated substrate and the member for discharging the hydrolyzed substrate at least in part are substantially vertical.
  • the sealed member for supplying impregnated substrate comprises an inlet valve and an outlet valve, means for level measurement inside the member, means for pressure balancing connected alternately to the pressurized hydrolysis reactor and to the atmosphere impregnation reactor and of the first means for controlling the level measurement means at the inlet and outlet valves of the supply member .
  • the sealed member for discharging the hydrolyzed substrate comprises an inlet valve and an outlet valve, second pressure balancing means connected alternately to the pressurized hydrolysis reactor and to the impregnation reactor for example which operates at atmospheric pressure and second means for controlling the inlet and outlet valves of the evacuation member to said second pressure balancing means.
  • the hydrolysis reactor can be inclined according to a downward slope of 0.1 to 1% directed towards the evacuation member, so as to recover any condensates.
  • the means for continuously transferring the impregnated substrate into the hydrolysis reactor can comprise an endless screw.
  • This endless screw can, according to a particularly advantageous embodiment, consist of a thick shaft with screw pitch tightened in the first quarter, for example, of its length and of a smaller shaft with larger screw pitch over the rest of its length. This configuration allows better distribution of the substrate and better regulation of the feed rate.
  • the apparatus makes it possible in particular to extract the lignin and to recover polymers based on easily hydrolyzable sugars.
  • the corn cobs after having been crushed in a conventional type of grinder 1, at an appropriate particle size, are sent using an elevator 2, for example with discs, to an impregnation reactor 5 via a gravimetric doser 3 supplying as a substrate, the inlet 4 of this reactor.
  • This substantially cylindrical reactor comprises an endless transfer screw 7 conveying the ground substrate to the outlet 10. This screw is controlled by a motor 6.
  • the acid supply flow is ensured by conventional injectors 8a arranged substantially annularly around the reactor, via a line 8 and a metering pump while the water flow is provided by injectors 9a identical to the injectors 8, arranged substantially annularly around the reactor and connected to a supply line 9 via a pump 9b.
  • injectors distribute their respective fluid substantially radially by means of pumps 8b, 9b and are advantageously located at a distance from the upstream end corresponding to a quarter of the length of the reactor.
  • First control and servo-control means make it possible to control the injection or supply flows in acid solution to the supply flow of ground substrate, to its dry matter content and to the speed of transfer in the reactor. such that the dry matter content of the stems goes from about 90% to about 50% and that there is substantially no separate liquid phase at the outlet 10 from the impregnation zone.
  • the stems are discharged by gravity and by an outlet perpendicular to the axis of the reactor 5 in a feed member 12 which is an airlock comprising an upper valve 18 called a guillotine valve in relation to the outlet 10 of the impregnation zone and a lower valve guillotine 19 which controls the entry of substrate into an acid hydrolysis reactor 11.
  • the latter of elongated shape , substantially cylindrical, and disposed in a substantially inclined downstream direction with a downward slope of approximately 0.5%, operates under pressure and at high temperature by means of the supply of water vapor injected substantially radially via a line 14.
  • the entry airlock arranged substantially vertically and substantially perpendicular to the axis of the reactor 11 comprises a level indicator 20 controlled by the first s control means 16 closing of a valve 18 when the airlock is sufficiently filled, pressurizing the airlock in equilibrium with the internal pressure of the hydrolysis reactor via a 3-way valve 21 and finally opening the valve 19 so that the contents of the airlock can flow into the hydrolysis reactor.
  • the 3-way valve 21 ensures successive alternative pressurization and atmospheric pressure.
  • the hydrolysis reactor 11 supplied with impregnated substrate ensures the transfer of the latter to the discharge member 15 by a transfer screw 13, set in motion by a motor 22.
  • This screw advantageously comprises a first part 22a over a distance corresponding to about a quarter of its length, consisting of a shaft with a larger diameter than that which comes in continuity on the second part 22b and with a pitch tighter than that of the second part.
  • the feed rates of impregnated substrate and of vapor and the speed of transfer into the hydrolysis zone are controlled by second control means 16 so that an at least partly hydrolyzed substrate is obtained which does not contain substantially no separate phase and a dry matter content lower than that which it had at the entry of the hydrolysis zone, for example 40 to 45%.
  • the pressure and the temperature of the hydrolysis reactor are regulated by sensors (not shown in the figure) and by the means 16 around a set value.
  • the setpoint value When the setpoint value is exceeded, the steam supply is stopped. However, it is open when the setpoint is not reached.
  • a solenoid valve 17 therefore controls the opening and closing of the steam supply 14 as a function of a signal delivered by the servo means 16 connected to the sensors.
  • the hydrolyzed substrate is then removed via an airlock 15 arranged vertically and substantially perpendicular to the axis of the hydrolysis reactor.
  • This airlock comprises an upper guillotine valve 23 and a lower guillotine valve 24 operating using the second servo means, the pressure balancing being effected by a 3-way valve 25 as already described in the case of the upper airlock.
  • the hydrolyzed substrate flows into a buffer tank 26, from which this same hydrolyzed substrate is recovered to supply a diffuser 27 performing continuously, in the presence of diffusion water supplied by a line 28, a solid liquid extraction against the current , the diffusion water first meeting the hydrolyzed substrate whose content of soluble sugars is practically completely exhausted.
  • the non-hydrolyzed organic material (lignin, cellulose) is recovered at one end 29 of the extraction line while the mixture of sugars in solution containing at least 80% by weight of xylose is recovered at the other end 30.
  • the mixture of sugars in solution is then concentrated, generally neutralized with lime, demineralized and discolored by passing, for example, through ion exchange resins.
  • Purified xylose (purity greater than 95%) can be obtained by crystallization from this solution of discolored sugars.
  • composition of the roundups is as follows: Humidity 9.0% Glucans 32.5% Xylans 28.8% Arabanes 3.7% Lignin 13.4% Ashes 2.0% Other constituents (including acetyl groups, uronic acids, etc.) 10.6%
  • the dry matter content at the exit from the impregnation zone is 50.6%.
  • the concentration by weight of acid relative to the dry matter is 4.0%.
  • the operating conditions of the hydrolysis reactor are 140 ° C. and a pressure of the order of 4 bar with an average residence time of 30 min.
  • the total quantity of product recovered at the outlet of the hydrolysis reactor is 1060 kg.
  • the material content of the hydrolyzed substrate is 42.9%.
  • the cobs having undergone the hydrolysis treatment are sent to a continuously operating diffuser in which the extraction of the sugars with water is carried out against the current.
  • An aqueous solution of sugars is recovered on the one hand and on the other hand stalks exhausted in monomeric sugars which are drained on a band filter, the filtrate then being added to the aqueous sugar solution, the final volume of which is 2200 liters. .
  • the total sugar content is 61.8 gl-1 with respective concentrations of xylose, glucose, arabinose of 51.8 gl-1, 5.4 gl-1 and 4.5 gl-1, i.e. a xylose content of 83.9%.
  • the aqueous solution is then evaporated under vacuum to reach a concentration of total sugars close to 150 g.l-1.
  • the evaporation temperature does not exceed 60 ° C. 920 l of a concentrated sugar solution are recovered, to which 10.1 kg of CaO are added.
  • the precipitate of calcium sulphate obtained is separated by filtration on a band filter.
  • the filtrate is then demineralized and discolored by passage over ion exchange resins and adsorbent resins.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)
  • Processing Of Solid Wastes (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Seasonings (AREA)

Claims (10)

  1. Verfahren zur kontinuierlichen Herstellung einer Zuckermischung in Lösung, welche wenigstens 80 % Xylose aus einem Lignozellulose-Rohstoff enthält und eine Stufe der Zerkleinerung, eine Stufe der Imprägnierung in wäßrig, saurer Lösung, eine Hydrolysestufe in Gegenwart von Wasserdampf, eine Stufe der Verdünnung in Gegenwart von Wasser, eine Stufe der Extraktion der aus dem Hydrolyserohstoff hergestellten Zuckermischung und eine Stufe der Rückgewinnung der Xylose umfaßt, gekennzeichnet durch die Verbindung der folgenden Stufen:
    a) man zerkleinert das Rohmaterial auf eine geeignete Größe,
    b) man speist kontinuierlich das Rohmaterial aus Stufe a) in eine Imprägnierungszone ein und bewirkt die Imprägnierungsstufe unter Bedingungen, daß man am Ausgang der Imprägnierungszone ein Rohmaterial mit einem derarten Trockengewicht, daß es keine separaten Flüssigphasen enthält, rückgewinnt,
    c) man speist kontinuierlich imprägniertes Rohmaterial aus der Sufe b) in eine Hydrolysezone unter Druck ein und und man bewirkt die Hydrolysestufe unter Bedingungen der Temperatur, des Druckes und des Wasserdampfaustritts, daß man ein wenigstens teilweise hydrolysiertes Rohmaterial, das keine separaten Phasen enthält, rückgewinnt.
  2. Verfahren nach Anspruch 1, worin die Imprägnierungsstufe mit einem Anteil an Säure, bezogen auf die Menge des Trockenmaterials des Rohmaterials, von 0,1 - 10 % bei Raumtemperatur und einem Druck, der dem Atmosphärendruck entspricht, während einer Minute bis 60 Minuten bewirkt wird.
  3. Verfahren nach Anspruch 1 bis 2, worin die Hydrolysestufe bei einer Temperatur von 120 bis 170°C bei einem Druck von 1 bis 7 Bar während 10 Minuten bis einer Stunde bewirkt wird.
  4. Verfahren nach einem der Ansprüche 1 bis 3, worin die Hydrolysestufe bei einer Temperatur von 135 bis 150°C bei 2 bis 5 Bar während 20 bis 40 Minuten bewirkt wird.
  5. Verfahren nach einem der Ansprüche 1 bis 4, worin der Gehalt des Trockenmateriales am Ausgang der Imprägnierungszone 30 bis 70 %, vorteilhaft 25 bis 55 %, beträgt.
  6. Verfahren nach einem der Ansprüche 1 bis 5, worin man das Rohmaterial der Hydrolysezone durch Schwerkraft einspeist.
  7. Einheit zur kontinuierlichen Herstellung, insbesondere von Xylose aus einem Lignozellulose - Rohstoff, welche Mittel zum Zerkleinern eines Rohstoffes auf geeignete Größe und Mittel zum Einspeisen zerkleinerten Rohmateriales umfaßt, dadurch gekennzeichnet, daß die Herstellungseinheit in Kombination einen Imprägnierungsreaktor für den zerkleinerten Rohstoff von zylindrischer Form mit einem Einlaß, der mit Mitteln zur Einspeisung des Rohstoffes leitend verbunden ist und einen Ausgang umfaßt, Mittel zur kontinuierlichen Überleitung des Rohstoffes in den Imprägnierungsreaktor und Mittel zur Einspeisung in Lösung, welche Wasser und wenigstens eine Säure oder wenigstens eine Base enthält, wobei der Imprägnierungsreaktor Reguliermittel, die mit Mitteln zur Rohstoffeinspeisung, mit Mitteln zur Überführung des Rohstoffes in den Imprägnierungsreaktor und mit Mitteln zur Einspeisung der Lösung verbunden sind, umfaßt und daran angepaßt ist, den Rohstoff unter Bedingungen zu imprägnieren, daß dieser frei von separaten Flüssigphasen ist, wobei die Herstellungseinheit weiters dadurch gekennzeichnet ist, daß sie einen kontinuierlich und unter Druck arbeitenden Hydrolysereaktor zylindrischer Form aus rostfreiem Stahl umfaßt, der an einem seiner Enden ein dichtes Organ zum kontinuierlichen Einspeisen des Rohstoffes umfaßt und mit dem Ausgang des Imprägnierungsreaktors leitend verbunden ist und daran angepaßt ist, entweder bei Raumdruck oder unter Druck zu arbeiten, Mittel zur kontinuierlichen Überführung des imprägnierten Rohstoffes in den Hydrolysereaktor, wenigstens ein Mittel zur Einspeisung von Dampf unter Druck und am anderen Ende ein dichtes Organ zur Evakuierung des hydrolysierten Rohstoffes, das daran angepaßt ist entweder bei atmosphärischem Druck oder unter Druck zu arbeiten und angepaßt ist ,darunter Extraktiosmittel der Zucker einzuspeisen, wobei der Hydrolysereaktor Reguliermittel, die mit den Einspeiseorganen für den Rohstoff und den Evakuierungsorganen für den Rohstoff, dem Ausstoß der Dampfeinspeisung und der Geschwindigkeit der Überleitung des Rohsoffes vebunden sind, wobei die Reguliermittel darauf eingestellt sind, den imprägnierten Rohstoff in Abwesenheit separater Flüssigphasen zu hydrolysieren, wobei die Einheit des weiteren Mittel zur kontinuierlichen Extraktion der Zucker umfaßt, welche insbesondere Xylose aus dem nichthydrolysierten Rohstoff enthalten, die mit dem Evakuierungsorgan verbunden sind und Mittel zur Wassereinspeisung und Mittel zur Rückgewinnung von Xylose, die verbunden mit Mitteln der Extraktion hergestellt ist, umfaßt.
  8. Herstellungseinheit nach Anspruch 7, worin der Hydrolysereaktor gemäß einem Gefälle von 0,1 bis 1 % gegen das Evakuierungsorgan geneigt ist.
  9. Herstellungseinheit nach Anspruch 7 oder 8, worin der Hydrolysereaktor eine Symmetrieachse aufweist und worin das Einspeisorgan und das Evakuierungsorgan des Rohstoffes senkrecht zur Symmetrieachse stehen.
  10. Herstellungseinheit nach einem der Ansprüche 7 bis 9, worin ein Pufferbehälter zwischen das Evakuierungsorgan und das Zucker-Extraktionsorgan geschaltet ist.
EP90403374A 1989-12-07 1990-11-28 Verfahren und Einrichtung zur Herstellung einer zumindest 80% Xylose enthaltende Zuckermischung aus einem lignocellulosischen Substrat Expired - Lifetime EP0432015B1 (de)

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Application Number Priority Date Filing Date Title
FR8916321A FR2655661B1 (fr) 1989-12-07 1989-12-07 Procede et unite de production en continu d'un melange de sucres contenant au moins 80% de xylose a partir d'un substrat lignocellulosique.
FR8916321 1989-12-07

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EP0432015A1 EP0432015A1 (de) 1991-06-12
EP0432015B1 true EP0432015B1 (de) 1994-10-26

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EP (1) EP0432015B1 (de)
DE (1) DE69013652T2 (de)
ES (1) ES2066173T3 (de)
FI (1) FI100254B (de)
FR (1) FR2655661B1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10759727B2 (en) 2016-02-19 2020-09-01 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1058996C (zh) * 1996-05-14 2000-11-29 安徽省科苑应用技术开发(集团)股份有限公司 由玉米芯提取木糖的改进方法
US6022419A (en) * 1996-09-30 2000-02-08 Midwest Research Institute Hydrolysis and fractionation of lignocellulosic biomass
FR3027821B1 (fr) 2014-10-31 2018-11-16 Centralesupelec Procede de purification d'oses.

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2413306B2 (de) * 1973-05-04 1976-09-30 Gebrüder Sulzer AG, Winterthur (Schweiz) Verfahren zum herstellen von xyloseloesung
CH585794A5 (de) * 1974-12-03 1977-03-15 Sulzer Ag
US4136207A (en) * 1977-01-24 1979-01-23 Stake Technology Ltd. Method of treating lignocellulose materials to produce ruminant feed
US4350766A (en) * 1980-08-01 1982-09-21 Purdue Research Foundation Pentose syrup production from hemicellulose
FR2580669B1 (fr) * 1985-04-18 1987-09-18 Inst Francais Du Petrole Procede de conversion de substrats lignocellulosiques en pentoses

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10759727B2 (en) 2016-02-19 2020-09-01 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources
US11840500B2 (en) 2016-02-19 2023-12-12 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources
US12139451B2 (en) 2016-02-19 2024-11-12 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources

Also Published As

Publication number Publication date
DE69013652D1 (de) 1994-12-01
EP0432015A1 (de) 1991-06-12
FR2655661B1 (fr) 1994-06-03
FI906037A0 (fi) 1990-12-05
DE69013652T2 (de) 1995-03-02
ES2066173T3 (es) 1995-03-01
FI100254B (fi) 1997-10-31
FI906037A7 (fi) 1991-06-08
FR2655661A1 (fr) 1991-06-14

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