WO1983001958A1 - Procede de production de pentose et d'hexose a partir d'un materiau cellulosique contenant des pentosanes au moyen d'une hydrolyse acide - Google Patents

Procede de production de pentose et d'hexose a partir d'un materiau cellulosique contenant des pentosanes au moyen d'une hydrolyse acide Download PDF

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Publication number
WO1983001958A1
WO1983001958A1 PCT/DK1982/000104 DK8200104W WO8301958A1 WO 1983001958 A1 WO1983001958 A1 WO 1983001958A1 DK 8200104 W DK8200104 W DK 8200104W WO 8301958 A1 WO8301958 A1 WO 8301958A1
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WO
WIPO (PCT)
Prior art keywords
pentose
xylose
hexose
acid
hydrolysis
Prior art date
Application number
PCT/DK1982/000104
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English (en)
Inventor
De Danske Sukkerfabrikker Aktieselskabet
De Danske Spritfabrikker Aktieselskabet
Original Assignee
Buus, Lasse
Nielsen, Werner, Kofod
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 Buus, Lasse, Nielsen, Werner, Kofod filed Critical Buus, Lasse
Priority to AU10169/83A priority Critical patent/AU1016983A/en
Publication of WO1983001958A1 publication Critical patent/WO1983001958A1/fr

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Classifications

    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • C13K1/02Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00Sugars not otherwise provided for in this class
    • C13K13/002Xylose

Definitions

  • This invention relates to a process for the production of pentose and hexose from a cellulosic material containing pentosans by -> 5 acid hydrolysis, said process comprising the step of heating the cel ⁇ lulosic material to an elevated temperature in the presence of a ? strong acid .
  • glucose can be prepared from various cellulosic materials, such as straw, sawdust, wood waste and sugar 10 cane bagasse, by heating the cellulosic material to an elevated tempe ⁇ rature in the presence of sulphuric acid .
  • Methods of this type have lately attracted considerable interest, partly because ' cellulosic raw materials are available in very large amounts and partly because there is a growing need for providing cheap glucose for use as a 15 starting material in the production of ethanol by fermentation .
  • hydrolysis of the pentosans to form xylose should also be carefully controlled in order to avoid that the hydrolysate, viz. xylose, is further converted into furfural .
  • the hydrolysis is effected at a tempe ⁇ rature of between 210 and 250°C for a period of between 5 and 90 seconds and in the presence of an acid having a concentration of from 0.2 to 2.0 % by weight.
  • the invention is based on the discovery that when using for example straw as starting material and by performing the hydro ⁇ lysis under the above mentioned operational conditions, it is possible to obtain a yield of xylose of about 50% (based on the amount of pentosans present in the starting material) together with a yield of glucose of above 50% (based on the amount of cellulose in the starting material).
  • the highest yields of xylose and glucose are obtained by effecting the hydrolysis at a temperature of from 225 to 235°C for a period of 30-60 seconds.
  • the reaction temperature and the reaction time should be carefully controlled and in a preferred embodiment of the method of the invention the acid hydrolysis is effected under pressure, e.g. at a pressure of 2-5 MPa in a tubular reactor and by heating the start ⁇ ing material by steam injection .
  • the reaction mixture can be rapidly heated and a corresponding rapid cooling can be effected by pressure relief, e. g . to atmospheric pressure.
  • the pressure- relieved product Is preferably further cooled or is neutral- ized by addition of base, such as Ca(OH) , in order to raise the pH value to 3 or above so as to stop the decomposition of glucose and xylose.
  • the neutralized product may then be filtered so as to form a filtrate containing xylose and glucose and a filter cake which option ⁇ ally after being dried is suitable as a solid fuel.
  • a filter cake which option ⁇ ally after being dried is suitable as a solid fuel.
  • the use of the filter cake as a solid fuel decreases the energy consumption of the process.
  • the filtrate may be separated into a xylose fraction and a glucose fraction but it is preferred to subject the filtrate to a fer ⁇ mentation before xylose is separated.
  • xylose is subse- quently separated, optionally in connection with part of the fermen ⁇ tation medium which is also suitable as animal feed together with the xylose.
  • the straw When using straw as starting material the straw is prefer ⁇ ably cut into pieces having a length of about 1-10 cm. When using other naturally occurring cellulosic materials containing pentosans, these should preferably be comminuted before the acid hydrolysis is started.
  • Examples of other suitable starting materials are sawdust, paper waste, bagasse, oat shells, corncobs and beet pulp.
  • the acid used is preferably a strong mineral acid, such as sulphuric acid, but also other mineral acids, such as hydrochloric acid are suitable.
  • Example 1 Barley straw was cut into lengths of about 1 cm and slurr ⁇ ed in a sulphuric acid solution .
  • the slurry thus obtained was pumped into a tubular reactor under a pressure of 3.2-4 MPa.
  • the temperature was raised to 230°C by direct injection of steam. After the injection of steam the acid concentration was 0.75%.
  • the tempera ⁇ ture was maintained for 30 seconds and then the pressure was sud ⁇ denly relieved to atmospheric pressure. As a result of said pressure relief a steam phase and an aqueous phase having a temperature of 100 C were formed .
  • the aqueous phase containing xylose and glucose was cooled to below 70°C.
  • Xylose was separated from the cooled aqueous phase in a yield of 63% (based on the weight of the pentosans present in the straw) and glucose was separated in a yield of 35% (based on the weight of the cellulose present in the straw) .
  • Example 3 The same procedure as described in Example 1 was used except that the reaction time was 41 seconds. The yield of xylose was 53% and the yield of glucose 41%.
  • Example 4 The same procedure as described in Example 1 was used, except that the concentration of the sulphuric acid solution was 0.63% and the reaction time was 45 seconds. The yield of xylose was 55% and the yield of glucose 48%.
  • Example 5 Barley straw was cut into lengths of about 3 cm and was pumped into a reactor under a pressure of 3.2-4 MPa. To the straw was added a sulfurlc acid solution of a temperature of 180 C and the mixture thus obtained was immediately heated to a temperature of 230 C by direct injection of steam . After the injection of steam the acid concentration was 0.8%. The temperature was maintained for 59 seconds and then the pressure was suddenly relieved to atmospheric pressure. As a result of said pressure relief a steam phase and an aqueous phase having a temperature of 100 C were formed . The aqueous phase containing xylose and glucose was cooled to below 70°C .
  • Xylose was recovered from the cooled aqueous phase in a yield of 18% (based on the weight of the pentosans present in the straw) and glucose was recovered in a yield of 53% (based on the weight of the cellulose present in the straw) .

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Saccharide Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Procédé de production de pentose et d'hexose à partir d'un matériau cellulosique contenant des pentosanes au moyen d'une hydrolyse acide, dans lequel le matériau de base est chauffé à une température comprise entre 210 et 250oC pendant une durée variable entre 5 et 90 secondes en présence d'un acide fort possédant une concentration comprise entre 0,2 et 2 % en poids. Un rendement élevé de production du pentose aussi bien que de l'hexose est obtenu par ce procédé à phase unique.
PCT/DK1982/000104 1981-11-25 1982-11-24 Procede de production de pentose et d'hexose a partir d'un materiau cellulosique contenant des pentosanes au moyen d'une hydrolyse acide WO1983001958A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU10169/83A AU1016983A (en) 1981-11-25 1982-11-24 Process for the production of pentose and hexose from a cellulosic material containing pentosans by acid hydrolysis

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DK5228/81811125 1981-11-25
DK522881A DK522881A (da) 1981-11-25 1981-11-25 Fremgangsmaade til omdannelse af et pentosanholdigt cellulosemateriale til xylose og glukose ved syrehydrolyse

Publications (1)

Publication Number Publication Date
WO1983001958A1 true WO1983001958A1 (fr) 1983-06-09

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DK1982/000104 WO1983001958A1 (fr) 1981-11-25 1982-11-24 Procede de production de pentose et d'hexose a partir d'un materiau cellulosique contenant des pentosanes au moyen d'une hydrolyse acide

Country Status (3)

Country Link
EP (1) EP0094958A1 (fr)
DK (1) DK522881A (fr)
WO (1) WO1983001958A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2580669A1 (fr) * 1985-04-18 1986-10-24 Inst Francais Du Petrole Procede de conversion de substrats lignocellulosiques en pentoses
US8568533B2 (en) 2011-05-04 2013-10-29 Renmatix, Inc. Multistage cellulose hydrolysis and quench with or without acid
US8747561B2 (en) 2011-05-04 2014-06-10 Renmatix, Inc. Cellulose hydrolysis with pH adjustment
US8840995B2 (en) 2011-05-04 2014-09-23 Renmatix, Inc. Lignin production from lignocellulosic biomass
US8968479B2 (en) 2010-01-19 2015-03-03 Renmatix, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
US9963555B2 (en) 2011-12-30 2018-05-08 Renmatix, Inc. Compositions comprising lignin
US10793646B2 (en) 2014-09-26 2020-10-06 Renmatix, Inc. Adhesive compositions comprising type-II cellulose

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3212933A (en) * 1963-04-12 1965-10-19 Georgia Pacific Corp Hydrolysis of lignocellulose materials with solvent extraction of the hydrolysate
EP0018348A1 (fr) * 1979-03-01 1980-10-29 Ruthner, Othmar, Dr. Dipl.-Ing. techn. Procédé et installation pour le traitement de déchets

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3212933A (en) * 1963-04-12 1965-10-19 Georgia Pacific Corp Hydrolysis of lignocellulose materials with solvent extraction of the hydrolysate
EP0018348A1 (fr) * 1979-03-01 1980-10-29 Ruthner, Othmar, Dr. Dipl.-Ing. techn. Procédé et installation pour le traitement de déchets

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2580669A1 (fr) * 1985-04-18 1986-10-24 Inst Francais Du Petrole Procede de conversion de substrats lignocellulosiques en pentoses
US8968479B2 (en) 2010-01-19 2015-03-03 Renmatix, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
US9359651B2 (en) 2010-01-19 2016-06-07 Renmatix, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
US10053745B2 (en) 2010-01-19 2018-08-21 Renmatix, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
US10858712B2 (en) 2010-01-19 2020-12-08 Renmatix, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
US8568533B2 (en) 2011-05-04 2013-10-29 Renmatix, Inc. Multistage cellulose hydrolysis and quench with or without acid
US8747561B2 (en) 2011-05-04 2014-06-10 Renmatix, Inc. Cellulose hydrolysis with pH adjustment
US8840995B2 (en) 2011-05-04 2014-09-23 Renmatix, Inc. Lignin production from lignocellulosic biomass
US9963555B2 (en) 2011-12-30 2018-05-08 Renmatix, Inc. Compositions comprising lignin
US10793646B2 (en) 2014-09-26 2020-10-06 Renmatix, Inc. Adhesive compositions comprising type-II cellulose

Also Published As

Publication number Publication date
EP0094958A1 (fr) 1983-11-30
DK522881A (da) 1983-05-26

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