EP0092478A1 - Procédé et dispositif d'hydrolyse d'une matière cellulosique - Google Patents

Procédé et dispositif d'hydrolyse d'une matière cellulosique Download PDF

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Publication number
EP0092478A1
EP0092478A1 EP83400747A EP83400747A EP0092478A1 EP 0092478 A1 EP0092478 A1 EP 0092478A1 EP 83400747 A EP83400747 A EP 83400747A EP 83400747 A EP83400747 A EP 83400747A EP 0092478 A1 EP0092478 A1 EP 0092478A1
Authority
EP
European Patent Office
Prior art keywords
extruder
hydrolysis
pressure
outlet
screws
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
EP83400747A
Other languages
German (de)
English (en)
French (fr)
Inventor
Maurice Gelus
Pierre Berger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Clextral SAS
Original Assignee
Clextral SAS
Creusot Loire SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Clextral SAS, Creusot Loire SA filed Critical Clextral SAS
Publication of EP0092478A1 publication Critical patent/EP0092478A1/fr
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B9/00—Presses specially adapted for particular purposes
    • B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
    • B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
    • B30B9/16—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing operating with two or more screws or worms
    • B30B9/163—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing operating with two or more screws or worms working in different chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B9/00—Presses specially adapted for particular purposes
    • B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
    • B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
    • B30B9/16—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing operating with two or more screws or worms
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials

Definitions

  • the subject of the invention is a method and a device for hydrolyzing a cellulosic material by passing it through an extruder.
  • the fragmented wood is treated with hydrochloric acid at 40% and the carbohydrate obtained is subjected to hydrolysis with dilute acid.
  • a percolation is carried out under pressure of the cellulosic material which passes against the current in several percolators placed in series.
  • the cellulosic material reduced in a divided form, from sawdust, for example, is introduced in the wet state at the upstream end of the barrel of an extruder comprising two parallel screws driven in rotation and which transport the material to the downstream end of the sheath. This is heated so that, in the downstream part, the transported material reaches a temperature of the order of 240 °. Water separates by evaporation and can be discharged through the upstream end. The material therefore becomes denser and gradually compresses during its downstream transport, the pressure in the outlet orifice being able to reach 35 bars.
  • the material undergoes intense kneading under the action of the screws, at the same time as a rise in temperature and pressure, and is brought into contact with a sulfuric acid solution introduced into the downstream part of the sheath.
  • the cellulose then very quickly transforms into glucose which is entrained towards the outlet orifice, the latter being closed by a valve or a valve intended to control the evacuation of the hydrolyzed material by maintaining the pressure at a value greater than the saturated vapor pressure of water at outlet temperature.
  • the quantity of water entrained downstream with the material remains in the form of a liquid phase in which the glucose formed by hydrolysis dissolves, constituting a syrup.
  • the mass of material discharged at the outlet therefore consists of solid residues containing lignin, associated with a liquid phase containing dissolved glucose and residual acid.
  • the plug thus formed at the downstream end of the sheath is discharged discontinuously by the valve into an expansion pot acting as a cyclone, in which a glucose paste containing sugars, lignin, cellulose having no cellulose is recovered. reacted, furfural and condensed water, most of the water escaping as vapor at the top of the trigger pot.
  • the subject of the invention is improvements to this process and a new installation at the outlet from which there is continuously obtained, on the one hand, a glucose syrup from which it is easy to extract the sugars and, on the other hand, a solid residue which does not containing only a small part of the sugars formed.
  • the device for controlling the evacuation under pressure of the hydrolyzed material consists of a second extruder disposed transversely to the hydrolysis extruder and also comprising at least two screws driven in rotation inside '' a sheath provided, in its central part, with an inlet orifice for the hydrolyzed material coming from the first extruder, at its downstream end, in the direction of transport of the screws, with an extrusion die for the evacuation of the solid face of the material in the form of a continuous plug which is impermeable to the pressure reached in the sheath and, at its upstream end, an orifice for evacuating the liquid phase expelled by compression and containing the dissolved glucose , said upstream orifice being provided with a regulator adjusted to a pressure higher than the saturated vapor pressure.
  • the extruder therefore comprises two parallel screws 11 and 12 driven in rotation by a motor not shown inside the sheath 1 which envelops them.
  • the latter is provided, at its upstream end in the direction of transport of the screws, with a supply orifice 13 through which the cellulosic material 2 is introduced, by means of a metering device 21.
  • screws whose structure allows defibration and / or washing of the lignocellulosic material, as described in French patents No. 2,319,737 and No. 2,451,763 deposited respectively on July 31, 1975 and March 22, 1979 by the same Company.
  • the cellulosic material 2 can be introduced into the extruder in the form of wood chips, as indicated in the previous patents already cited.
  • heating or cooling chambers 14 which make it possible to adjust the temperature rise from upstream to downstream, this one having to reach a value of the order of 240 ° C. downstream end.
  • a dilute acid solution normally sulfuric acid
  • a line 3 provided with a metering pump 30, from a reservoir 31.
  • a line 32 makes it possible to introduce a liquid phase or water vapor near the outlet of the extruder, to adjust, if necessary, the temperature of the material and the humidity rate.
  • the material introduced through the orifice 13 and containing for example 30% by weight of water, is transported downstream by the rotation of the screws 11 and 12 and is subjected to intense mixing, to progressive compression and at the same time at a rise in temperature.
  • Most of the water can be evacuated in the form of vapor by the upstream end and by the inlet orifice 13, another part being entrained with the solid phase.
  • the two screws 11 and 12 are provided with a braking zone 15 which can be made up of threads with tightened or inverted pitch preferably provided with windows 150 allowing a controlled flow of material to flow downstream, so as to cause a rise in pressure of the material up to a determined value.
  • the material can reach, for example, a pressure greater than 30 bars.
  • the temperature being of the order of 240 ° C., this pressure is greater than the saturation vapor pressure of the water, which thus remains mixed in liquid form with the solid residues constituted essentially by lignin.
  • the glucose formed by hydrolysis remains dissolved inside the extruded mixture.
  • the hydrolysis extruder 1 opens at its outlet 16, in the middle part of a second extruder 4 disposed transversely to the first and comprising a sheath 40 inside which are driven in rotation of two parallel screws 41 and 42 whose axes are preferably placed in a plane perpendicular to the axes of the two screws 11 and 12.
  • the sleeve 40 is provided at its downstream end, in the direction of transport of the screws, with an extrusion die 43 and constitutes a pressure-tight enclosure prevailing in the outlet orifice 16, the passages of the shafts of the two screws 41 and 42 being in particular provided with seals 49.
  • the sheath 40 At its other end, upstream from the orifice 16, the sheath 40 is provided on the other hand with an orifice 44 to which a pipe is connected evacuation 45 which is connected to an expansion pot 5 by means of a regulator 50.
  • the two screws 41 and 42 are provided, at their downstream ends, with threads with inverted pitch 46 provided with windows 460 allowing a controlled flow of material to pass downstream. In this way the pressure rises to a value which can be between 80 and 150 bars.
  • the glucose paste exiting through the orifice 16 and supported by the screws 41, 42 of the outlet extruder 4 is subjected therein to phase separation, the solid phase being entrained towards the downstream while the liquid phase is expelled and comes to concentrate in the upstream part 47 of the extruder 4.
  • This effect is due in particular to the use of an extruder with two preferably identical screws and rotated in the same direction .
  • the regulator 50 is adjusted to maintain the pressure in the barrel 40 at a value greater than the saturated vapor pressure so that the syrup is in the liquid phase.
  • a pressure gauge 51 allows the pressure to be checked and the regulator 50 to be adjusted accordingly.
  • the hydrolysis extruder 1 can be adjusted taking into account only the conditions for carrying out the hydrolysis reaction, the pressure being maintained by the outlet extruder 4 and determined by the adjustment of the regulator 50; the speed of the screws of the extruder 4 is permanently adjusted to adjust to the viscosity and the flow rate of the material leaving the orifice 16 in order to obtain in the die 43 a plug of compressed material sealed to the pressure prevailing in the extruder 4.
  • the wrung material leaving it contains only a very small quantity of sugar which can be recovered later, most of the glucose remaining dissolved in the syrup which is evacuated via line 45 into the jar trigger 5.
  • the liquid phase evaporates and is evacuated by the chimney 52 while the solution condenses on the walls of the trigger pot 5. It can thus establish an equilibrium regime, the conditions being adjusted separately in each screw by monitoring the various parameters, temperature pressure, concentration of syrup at the outlet, viscosity and water content of solid residues etc ...
  • the phase separation carried out, according to the invention, in the output extruder 4 also has the advantage of removing almost as soon as it is formed, the sugar contained in the liquid phase from the lignin contained in the solid phase and thus reducing the risk of reversal of the reaction which can occur, to a certain extent, in the other processes, when the sugar formed remains too long under the conditions of the hydrolysis reaction.
  • the temperature of the evacuated solid phase can thus be adjusted to further reduce the risk of reversing the reaction if it is feared that the residence time exceeds a fixed limit, for example 20 seconds.
  • liquid phase contained in the upstream part can be cooled to facilitate expansion while maintaining the pressure at the desired value.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
EP83400747A 1982-04-15 1983-04-15 Procédé et dispositif d'hydrolyse d'une matière cellulosique Ceased EP0092478A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8206473 1982-04-15
FR8206473A FR2525236A1 (fr) 1982-04-15 1982-04-15 Procede et dispositif d'hydrolyse d'une matiere cellulosique

Publications (1)

Publication Number Publication Date
EP0092478A1 true EP0092478A1 (fr) 1983-10-26

Family

ID=9273043

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83400747A Ceased EP0092478A1 (fr) 1982-04-15 1983-04-15 Procédé et dispositif d'hydrolyse d'une matière cellulosique

Country Status (6)

Country Link
US (1) US4478644A (enrdf_load_stackoverflow)
EP (1) EP0092478A1 (enrdf_load_stackoverflow)
BR (1) BR8301900A (enrdf_load_stackoverflow)
CA (1) CA1193251A (enrdf_load_stackoverflow)
FR (1) FR2525236A1 (enrdf_load_stackoverflow)
NZ (1) NZ203904A (enrdf_load_stackoverflow)

Families Citing this family (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4591386A (en) * 1981-04-17 1986-05-27 New York University Continuous apparatus for chemical conversion of materials
US4637835A (en) * 1985-06-28 1987-01-20 Power Alcohol, Inc. Methods of hydrolyzing cellulose to glucose and other (poly)saccharides
US4965086A (en) * 1988-01-04 1990-10-23 Degussa Aktiengesellschaft Chemical-mechanical treatment of lignocellulosics to improve nutritive value
US5023097A (en) * 1988-04-05 1991-06-11 Xylan, Inc. Delignification of non-woody biomass
US4842877A (en) * 1988-04-05 1989-06-27 Xylan, Inc. Delignification of non-woody biomass
US5972118A (en) * 1995-10-27 1999-10-26 Tennessee Valley Authority Concentrated sulfuric acid hydrolysis of lignocellulosics
US6022419A (en) * 1996-09-30 2000-02-08 Midwest Research Institute Hydrolysis and fractionation of lignocellulosic biomass
US5876505A (en) * 1998-01-13 1999-03-02 Thermo Fibergen, Inc. Method of producing glucose from papermaking sludge using concentrated or dilute acid hydrolysis
US20050166812A1 (en) * 2003-11-13 2005-08-04 Horizon Fuel And Financial Management, Llp MSW processing vessel
US7967877B2 (en) * 2003-11-13 2011-06-28 Biomass Worldwide Group Limited Biomass energy product and processing method
BRPI0516755A (pt) * 2004-09-30 2008-09-16 Iogen Energy Corp processo contìnuo para o pré-tratamento de uma carga de alimentação lignocelulósica
US8728802B2 (en) * 2006-02-15 2014-05-20 Biomass Worldwide Group Limited Angled reaction vessel
US7745208B2 (en) * 2006-02-15 2010-06-29 Noll Anthony P Angled reaction vessel
US7815741B2 (en) 2006-11-03 2010-10-19 Olson David A Reactor pump for catalyzed hydrolytic splitting of cellulose
US7815876B2 (en) * 2006-11-03 2010-10-19 Olson David A Reactor pump for catalyzed hydrolytic splitting of cellulose
US20130239955A1 (en) * 2010-11-25 2013-09-19 Ferdi Schüth Method for the acid-catalyzed depolymerization of cellulose
JP6188807B2 (ja) * 2012-09-20 2017-08-30 ノラム エンジニアリング アンド コンストラクターズ リミテッド 圧縮セルロース系材料を使用する部分的に加水分解されたセルロースを製造する方法
US9809867B2 (en) 2013-03-15 2017-11-07 Sweetwater Energy, Inc. Carbon purification of concentrated sugar streams derived from pretreated biomass
EP3230463B2 (en) 2014-12-09 2025-07-16 Apalta Patents OÜ Rapid pretreatment
WO2018151833A1 (en) 2017-02-16 2018-08-23 Sweetwater Energy, Inc. High pressure zone formation for pretreatment
CA3165573A1 (en) 2019-12-22 2021-07-01 Sweetwater Energy, Inc. Methods of making specialized lignin and lignin products from biomass
EP3885105A1 (en) * 2020-03-25 2021-09-29 Admatec Europe B.V. Pellet extruder for 3d printing

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2472016A1 (fr) * 1979-12-18 1981-06-26 Tampella Oy Ab Procede de saccharification continue de la cellulose de plantes
EP0037912A2 (en) * 1980-03-18 1981-10-21 New York University Process and apparatus for chemical conversion of cellulose waste to glucose

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2681871A (en) * 1951-02-16 1954-06-22 Sam M Nickey Jr Method and apparatus for hydrolyzing cellulosic materials
US3947169A (en) * 1966-07-29 1976-03-30 Allied Chemical Corporation Apparatus for making rods or tubes having a filter
BE790700A (fr) * 1971-11-18 1973-04-27 Rohm & Haas Perfectionnements aux procedes pour purifier et melanger des polymeres
US4316747A (en) * 1980-03-18 1982-02-23 New York University Process for the chemical conversion of cellulose waste to glucose
DE3108823A1 (de) * 1981-03-09 1982-09-16 Hermann Berstorff Maschinenbau Gmbh, 3000 Hannover "einrichtung zur kontinuierlichen herstellung von glucose enthaltenden produkten"

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2472016A1 (fr) * 1979-12-18 1981-06-26 Tampella Oy Ab Procede de saccharification continue de la cellulose de plantes
EP0037912A2 (en) * 1980-03-18 1981-10-21 New York University Process and apparatus for chemical conversion of cellulose waste to glucose

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
CHEMICAL & ENGINEERING NEWS, 8 octobre 1979, pages 19-20, USA *
CHEMICAL ABSTRACTS, vol. 96, no. 12, 22 mars 1982, page 97, no. 87247q, Columbus, Ohio, USA *
CHEMICAL ABSTRACTS, vol. 97, no. 12, 20 septembre 1982, page 193, no. 95434j, Columbus, OHio, USA *
SOVIET INVENTIONS ILLUSTRATED SECTION CH: CHEMICAL, week D05, 11 mars 1981, page 9, Derwent Publications Ltd., London, GB. & SU - A - 737 461 (G.V. CHERNYKH) 06-04-1977 *

Also Published As

Publication number Publication date
US4478644A (en) 1984-10-23
NZ203904A (en) 1985-11-08
FR2525236A1 (fr) 1983-10-21
BR8301900A (pt) 1983-12-20
CA1193251A (fr) 1985-09-10
FR2525236B1 (enrdf_load_stackoverflow) 1984-06-01

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PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

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Effective date: 19831018

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Effective date: 19860317

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Inventor name: BERGER, PIERRE

Inventor name: GELUS, MAURICE