EP0081678A2 - Procédé et dispositif pour l'hydrolyse de la cellulose - Google Patents

Procédé et dispositif pour l'hydrolyse de la cellulose Download PDF

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Publication number
EP0081678A2
EP0081678A2 EP82110340A EP82110340A EP0081678A2 EP 0081678 A2 EP0081678 A2 EP 0081678A2 EP 82110340 A EP82110340 A EP 82110340A EP 82110340 A EP82110340 A EP 82110340A EP 0081678 A2 EP0081678 A2 EP 0081678A2
Authority
EP
European Patent Office
Prior art keywords
steam
reaction
stage
preheating chamber
reactor vessel
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.)
Granted
Application number
EP82110340A
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German (de)
English (en)
Other versions
EP0081678A3 (en
EP0081678B1 (fr
Inventor
Klaus-Jürgen Dr. Hinger
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.)
Werner and Pfleiderer GmbH
Original Assignee
Werner and Pfleiderer GmbH
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 Werner and Pfleiderer GmbH filed Critical Werner and Pfleiderer GmbH
Priority to AT82110340T priority Critical patent/ATE18435T1/de
Publication of EP0081678A2 publication Critical patent/EP0081678A2/fr
Publication of EP0081678A3 publication Critical patent/EP0081678A3/de
Application granted granted Critical
Publication of EP0081678B1 publication Critical patent/EP0081678B1/fr
Expired legal-status Critical Current

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Classifications

    • 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 invention relates to a method according to the preamble of claim 1 and an apparatus for performing this method.
  • Alcohol for such purposes can be made from cellulose or cellulosic biomass in two stages by first hydrolyzing cellulose to sugar and then fermenting it to ethanol. While the fermentation of sugar to ethanol is technically well mastered, the hydrolysis of cellulose remains the critical process step that decides on the overall economy of the process.
  • the invention has for its object to provide a method and apparatus by which high yields of fermentable sugar relative to the employed Cellulose from about 6 0% can be achieved, through which the energy requirement as small as possible, in particular o, 5 kg of steam per kg of dry matter and less than o, ol kWh of drive energy per kg of dry matter is held by which the investment costs remain within a reasonable range and ultimately an environmental friendliness of the process itself and the by-products to be eliminated is guaranteed.
  • the temperature parameter can be freely selected over a wide range if only the corresponding decrease in the reaction time with increasing temperature is ensured.
  • the number of reaction stages is dimensioned such that the ratio of to the setting for the respective stage characteristic data on the reaction time of this stage is sufficiently high and remains sufficiently manageable within the framework of an industrial process.
  • reaction temperature and duration given there also makes it possible to set the temperature stages in such a way that reaction times which are technically manageable result.
  • a device according to claim 5 is used to carry out the method described above.
  • a fluidized bed reactor provided thereafter creates the conditions for the short to very short reaction times desired according to the invention, since the reaction times of the stage can be set very quickly there.
  • the waste heat can be advantageously used and by assigning it to the actual reaction vessel there are very short transport routes for the products to be subjected to hydrolysis.
  • Claim 7 shows a particularly favorable possibility of feeding the starting material, which in particular also enables quasi-continuous operation.
  • the stripping devices provided according to claim 9 eliminate cellulose residues which stick to the actuating rod in the preheating chamber during the preheating process.
  • water showers can also be provided for cleaning the valve closing parts.
  • An embodiment according to claim 10 also ensures that the material to be hydrolyzed is fluidized in the reactor vessel and is surrounded on all sides by condensing water vapor. This avoids the formation of lumps, which would increase the heating times.
  • the rapid relaxation important for kinetic reasons is also promoted at the end of each cycle stage.
  • the rate of expansion may at most be such that no hydrolysis product or remaining starting material escapes from the reactor vessel through the steam discharge line.
  • the embodiment according to claim 12 enables in particular the implementation of the live steam-saving method step according to claim 3, which applies accordingly to the measure of claim 13 with regard to the procedural procedure according to claim 4.
  • the material to be hydrolyzed e.g. B. waste paper, residual wood, straw and. Like., First crushed in a known manner, then impregnated in a dilute sulfuric acid or other suitable acid solution of 0.5 to 10%, then mechanically dewatered to 10 to 80% by weight of moisture and then loosely re-crushed in a form
  • Preheating chamber poured into a reactor vessel.
  • the starting material is heated from room temperature to 100 ° C. by condensation of the steam by means of steam from a previous reaction stage pass. The material is then passed from the preheating chamber into the actual reactor vessel.
  • a first reaction stage I the cellulose conversion is allowed to rise from 0 to 4% at a temperature of 175 ° C. for a reaction time of 40 seconds.
  • stage II the conversion at a temperature of 225 ° C. during a reaction time of 4.5 seconds is increased from 4% to 30%, and finally the conversion in stage III at a temperature of 260 ° C. during a reaction time increased from 1.3% from 85% to 85%.
  • stage III After the end of the reaction in the last stage III, the temperature is rapidly lowered by releasing the steam in the reaction vessel in order to prevent a further reaction which would preferably decompose the sugar formed.
  • the amount of steam required to heat the material from state b to c and to pressurize the reactor to pressure P3 is the same as that which is released during the expansion from state d to state c.
  • a second steam accumulator in state c is therefore able to supply the heating steam required for state change b - d from the expansion steam fed in from state change d - c.
  • the amount of steam required to heat the material from state c to d and to pressurize the reactor vessel to pressure P 4 must be supplied by a steam generator. Its pressure p 5 is suitably very high, z. B. 100 bar, so that the heating time from state c to d is very short compared to the reaction time.
  • the exhaust steam from the last expansion stage, the change in state from b to a, is used to preheat the material impregnated with acid in the preheating chamber. After warming up, a new full reaction stage run can begin.
  • a device shown in FIG. 1 is used to carry out the method according to the invention.
  • This comprises a section of concave reactor vessel 1.
  • This is designed as a high pressure vessel.
  • the inside of the vessel 1 is coated with an acid-resistant, poorly heat-conducting material, such as ceramic, in order to avoid the condensation of water vapor and the resulting losses as far as possible.
  • thermal insulation not shown in the drawing, is provided.
  • a preheating chamber 2 is arranged above the reactor vessel 1. This is connected to the reactor vessel 1 via an inlet opening 3.
  • the inlet opening 3 is closed by a movable valve closing part 4, which is shown in dashed lines in its open position.
  • stripping devices 8 are provided for stripping residues of the starting material which are adhered there and which are actuated via hydraulic or pneumatic drive devices 9.
  • an outlet opening 10 is provided, which is closed by a valve closing part 11, the open position of which is also shown in dashed lines.
  • the valve closing part 11 is connected via an actuating rod 12 to a hydraulic or pneumatic actuating device 13, the actuating rod 12 passing through a product outlet channel 14 ′ adjoining the outlet opening 10.
  • Valve closing part 11, actuating rod 12 and actuating device 13 together form an outlet valve 14.
  • the preheating chamber 2 has a feed opening 15 on the side, to which a horizontal channel 16 with a plunger 17 which is longitudinally movable and sealingly guided is connected.
  • a funnel-shaped lower part 18 of a material storage container 19 opens into the channel 16 from above.
  • An annular nozzle channel 20 with a plurality of steam inlet nozzles 21 is provided on the reactor vessel 1 below the closing part 4 of the inlet valve 7.
  • the ring nozzle channel 20 is connected to a steam outlet opening 22 and a steam outlet line 23.
  • a line 24 leads from the steam outlet line 23 via a shut-off device 25 to the preheating chamber 2, while the steam outlet line 23 is in turn connected to steam pressure storage devices 26 and 27.
  • Shut-off devices 28 and 29 are assigned to the steam pressure storage devices 26 and 27.
  • a second ring nozzle channel 30 is located in the reactor vessel 1 above the closing part 11 of the outlet valve 14 and is connected to a steam inlet opening 31 and a steam inlet line 32.
  • the steam inlet line 32 is connected via shut-off devices 33 and 34 and 35 on the one hand to an unillustrated fresh steam source and on the other hand to the steam pressure storage devices 26 and 27.
  • the device according to the invention is operated such that the material pre-impregnated, dewatered and shredded cellulose-containing material is filled into the material storage container 19.
  • the funnel-shaped lower part 18 acts together with the channel 16 as a metering trough, which is delimited by the plunger 17 in FIG. 1 in the starting position on the right.
  • the material is pushed into the preheating chamber 2 by a longitudinal movement of the plunger 17 Intake valve 7 is in the closed position. In the end position, the plunger 17 closes the feed opening 15. No special requirements need be made of the quality of this seal.
  • reaction vessel 1 the reaction stages now take place in the manner described above, in that steam is fed in succession from the steam pressure storage devices 26 and 27 via the inlet line 32 and finally live steam by opening the shut-off device 33.
  • the steam added in each case flows in via the ring nozzle channel 30, so that the material to be hydrolyzed is fluidized in the reaction vessel.

Landscapes

  • Chemical & Material Sciences (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)
EP82110340A 1981-12-15 1982-11-10 Procédé et dispositif pour l'hydrolyse de la cellulose Expired EP0081678B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82110340T ATE18435T1 (de) 1981-12-15 1982-11-10 Verfahren und vorrichtung zur hydrolytischen spaltung von cellulose.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19813149587 DE3149587A1 (de) 1981-12-15 1981-12-15 Verfahren und vorrichtung zur hydrolytischen spaltung von cellulose
DE3149587 1981-12-15

Publications (3)

Publication Number Publication Date
EP0081678A2 true EP0081678A2 (fr) 1983-06-22
EP0081678A3 EP0081678A3 (en) 1984-05-09
EP0081678B1 EP0081678B1 (fr) 1986-03-05

Family

ID=6148743

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82110340A Expired EP0081678B1 (fr) 1981-12-15 1982-11-10 Procédé et dispositif pour l'hydrolyse de la cellulose

Country Status (8)

Country Link
US (1) US4708746A (fr)
EP (1) EP0081678B1 (fr)
JP (1) JPS58141799A (fr)
AT (1) ATE18435T1 (fr)
BR (1) BR8207282A (fr)
DE (2) DE3149587A1 (fr)
SU (1) SU1449013A3 (fr)
ZA (1) ZA827528B (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4992105A (en) * 1987-09-03 1991-02-12 Werner & Pfleiderer, Gmbh Method and apparatus for the hydrolytic separation of cellulose
US6418875B1 (en) 2000-04-07 2002-07-16 Koninklijke Philips Electronics N.V. Method of improving adhesion of cap oxide to nanoporous silica for integrated circuit fabrication
WO2012097781A1 (fr) * 2010-11-25 2012-07-26 Studiengesellschaft Kohle Mbh Procédé de dépolymérisation de cellulose, catalysée par de l'acide
WO2014139515A2 (fr) 2013-03-12 2014-09-18 Studiengesellschaft Kohle Mbh Procédé de dégradation de biomasse lignocellulosique

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5788983A (en) * 1989-04-03 1998-08-04 Rutgers, The State University Of New Jersey Transdermal controlled delivery of pharmaceuticals at variable dosage rates and processes
NZ229080A (en) * 1989-05-11 1991-10-25 Convertech Group Ltd Two stage process and equipment for the steam hydrolysis of woody material
US5411594A (en) * 1991-07-08 1995-05-02 Brelsford; Donald L. Bei hydrolysis process system an improved process for the continuous hydrolysis saccharification of ligno-cellulosics in a two-stage plug-flow-reactor system
US5198074A (en) * 1991-11-29 1993-03-30 Companhia Industreas Brasileiras Portela Process to produce a high quality paper product and an ethanol product from bamboo
NZ248895A (en) * 1993-10-08 1995-07-26 Convertech Group Ltd Transfer device having intermittently rotated carousel having through passageways with assembly sealing pressure maximised during rotor dwell periods
US6022419A (en) * 1996-09-30 2000-02-08 Midwest Research Institute Hydrolysis and fractionation of lignocellulosic biomass
US6228177B1 (en) 1996-09-30 2001-05-08 Midwest Research Institute Aqueous fractionation of biomass based on novel carbohydrate hydrolysis kinetics
BR9902606B1 (pt) * 1999-06-23 2011-04-19 combustìvel de celulignina catalìtica.
US7604967B2 (en) * 2003-03-19 2009-10-20 The Trustees Of Dartmouth College Lignin-blocking treatment of biomass and uses thereof
US8580541B2 (en) * 2003-03-19 2013-11-12 The Trustees Of Dartmouth College Lignin blockers and uses thereof
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
US8057639B2 (en) * 2008-02-28 2011-11-15 Andritz Inc. System and method for preextraction of hemicellulose through using a continuous prehydrolysis and steam explosion pretreatment process
DE102009010233B4 (de) * 2009-02-24 2020-06-10 Revatec Gmbh Verfahren zum Erzeugen von Kohle aus Biomasse
AP3563A (en) * 2009-09-29 2016-01-27 Nova Pangaea Technologies Ltd Method and system for fractionation of lignocellulosic biomass
WO2011103180A2 (fr) * 2010-02-16 2011-08-25 Grain Processing Corporation Procédé pour l'hydrolyse de fibres humides et procédé pour la production de produits de fermentation à partir de fibres humides
US20160046731A1 (en) * 2014-08-14 2016-02-18 Api Intellectual Property Holdings, Llc Production of sugars from biomass using solid catalysts
GB2602882B (en) * 2021-11-22 2023-03-29 Mostex Global Solutions Ltd Biomass steam explosion apparatus

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1007264A (fr) * 1948-03-12 1952-05-05 Traitement de produits végétaux à haute pression, production de sucres, furfurol, extraits tanniques et aliments pour bétail
DD130582A1 (de) * 1977-01-20 1978-04-12 Siegfried Poller Verfahren und vorrichtung zur hydrolyse von zellulosehaltigen materialien,insbesondere holz
EP0054871A1 (fr) * 1980-12-23 1982-06-30 Werner & Pfleiderer Procédé pour l'hydrolyse de la cellulose à partir de matières végétales en glucose et dispositif pour la mise en oeuvre de ce procédé

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2356500A (en) * 1941-03-27 1944-08-22 Boinot Firmin Charles Method for saccharifying cellulosic materials by means of diluted mineral acids
DE1567335C3 (de) * 1967-10-17 1979-03-29 Rudolf Dipl.-Ing. 8000 Muenchen Eickemeyer Verfahren und Vorrichtung zum chemischen Aufschluß cellulosehaltigen Materials
DE2803465A1 (de) * 1978-01-27 1979-08-02 Hans Dipl Ing Knauth Verfahren zur erzeugung von zellstoff aus pflanzlichen faserrohstoffen unter verwendung organischer loesungsmittel - hydrosolvverfahren
NZ191061A (en) * 1978-07-27 1982-03-16 Obbola Linerboard Ab Chemical pulp manufacture cellulosic material preheated by steam in a storage container
US4461648A (en) * 1980-07-11 1984-07-24 Patrick Foody Method for increasing the accessibility of cellulose in lignocellulosic materials, particularly hardwoods agricultural residues and the like
SE422604B (sv) * 1980-08-29 1982-03-15 Modo Chemetics Ab Forfarande for flidforvermning

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1007264A (fr) * 1948-03-12 1952-05-05 Traitement de produits végétaux à haute pression, production de sucres, furfurol, extraits tanniques et aliments pour bétail
DD130582A1 (de) * 1977-01-20 1978-04-12 Siegfried Poller Verfahren und vorrichtung zur hydrolyse von zellulosehaltigen materialien,insbesondere holz
EP0054871A1 (fr) * 1980-12-23 1982-06-30 Werner & Pfleiderer Procédé pour l'hydrolyse de la cellulose à partir de matières végétales en glucose et dispositif pour la mise en oeuvre de ce procédé

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
INDUSTRIAL & ENGINEERING CHEMISTRY PRODUCT RESEARCH AND DEVELOPMENT, Band 18, Nr. 3, September 1979, Seiten 166-169, American Chemical Society, US *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4992105A (en) * 1987-09-03 1991-02-12 Werner & Pfleiderer, Gmbh Method and apparatus for the hydrolytic separation of cellulose
US6418875B1 (en) 2000-04-07 2002-07-16 Koninklijke Philips Electronics N.V. Method of improving adhesion of cap oxide to nanoporous silica for integrated circuit fabrication
WO2012097781A1 (fr) * 2010-11-25 2012-07-26 Studiengesellschaft Kohle Mbh Procédé de dépolymérisation de cellulose, catalysée par de l'acide
EA023989B1 (ru) * 2010-11-25 2016-08-31 Штудиенгезельшафт Коле Мбх Способ кислотно-катализируемой деполимеризации целлюлозы
WO2014139515A2 (fr) 2013-03-12 2014-09-18 Studiengesellschaft Kohle Mbh Procédé de dégradation de biomasse lignocellulosique
DE102014102972A1 (de) 2013-03-12 2014-09-18 Studiengesellschaft Kohle Mbh Verfahren zum Aufschluss lignocellulosischer Biomasse

Also Published As

Publication number Publication date
ZA827528B (en) 1983-08-31
BR8207282A (pt) 1983-10-18
US4708746A (en) 1987-11-24
SU1449013A3 (ru) 1988-12-30
ATE18435T1 (de) 1986-03-15
EP0081678A3 (en) 1984-05-09
JPS58141799A (ja) 1983-08-23
EP0081678B1 (fr) 1986-03-05
DE3149587A1 (de) 1983-06-23
DE3269694D1 (en) 1986-04-10

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