EP0056409B1 - Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux - Google Patents

Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux Download PDF

Info

Publication number
EP0056409B1
EP0056409B1 EP19810902305 EP81902305A EP0056409B1 EP 0056409 B1 EP0056409 B1 EP 0056409B1 EP 19810902305 EP19810902305 EP 19810902305 EP 81902305 A EP81902305 A EP 81902305A EP 0056409 B1 EP0056409 B1 EP 0056409B1
Authority
EP
European Patent Office
Prior art keywords
cooking
alcohol
metal salt
delignification
earth metal
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.)
Expired
Application number
EP19810902305
Other languages
German (de)
English (en)
Other versions
EP0056409A1 (fr
Inventor
Laszlo Paszner
Pei-Ching Chang
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.)
Bau und Forschungsgesellschaft Thermoform AG
Original Assignee
Bau und Forschungsgesellschaft Thermoform AG
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 Bau und Forschungsgesellschaft Thermoform AG filed Critical Bau und Forschungsgesellschaft Thermoform AG
Priority to AT81902305T priority Critical patent/ATE54190T1/de
Publication of EP0056409A1 publication Critical patent/EP0056409A1/fr
Application granted granted Critical
Publication of EP0056409B1 publication Critical patent/EP0056409B1/fr
Expired legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment

Definitions

  • the invention relates to a method for the digestion of lignocellulose material to recover a fibrous cellulose by dissolving the lignin and hemicellulose constituents of the lignocellulose material in an aqueous methyl or ethyl alcohol containing dissolved a chloride or nitrate of magnesium, calcium or barium or magnesium sulfate or a mixture thereof in an amount of from 0.001 to 1.0 molar, for not more than two hours at elevated temperatures above 130°C and pressures, the amount of cooking liquor being at least 4 parts by weight per part by weight of the lignocellulose material, and recovery of the cellulose which has remained undissolved.
  • the problem to be solved by the invention is to improve delignification specificity for all lignocellulose species and thereby to increase the yield of cellulose pulp, to reduce viscosity losses in cellulose due to carbohydrate degradation, improve the quality and stability of dissolved lignin in solution and increase the uniformity of digestion at reduced cooking times of air-dry softwood chips and increase temperature stability of lignocellulose materials during high temperature digestion.
  • the effect of the additive is much greater than with the addition of either the alkaline earth metal salt or the acid reacting substances, so that the total amount of additives can be substantially reduced.
  • methanol is the preferred alcohol, but where methanol is not available in sufficient amount ethanol can be used as well.
  • the alcohol content of the cooking liquor must be between 80 and 98 percent by volume, but the higher percentages within this range are relatively difficult to achieve because of the moisture contained in the lignocellulose starting material.
  • the preferred ratio of lignocellulose material to cooking liquor is 1:6 to 1:20 by weight.
  • Wood chips in both air-dry and green conditions were conditioned to a uniform moisture content before the pulping trials.
  • Batch quantities of commercial size chips were charged into the digester with ten times their weight of cooking liquor containing predetermined quantities of the salt catalysts.
  • the volume ratio of methanol to water ranged between 90:10.
  • the sealed stationary vessel was quickly brought to cooking temperature in a thermostatically controlled glycerine bath and the temperature held constant for the cooking interval required.
  • the reported cooks are those which at the end of the stated period produced a free pulp when slurried in a disintegrator at slow stirred speed.
  • the pulping liquor when subjected to vacuum distillation at low temperature yields a flocculated lignin precipitate.
  • a sugar solution having a solids concentration up to 25 per cent by weight is obtained.
  • Charcoal filtration removes most of the yellow color due to the water soluble lignin depolymerisation products.
  • the molecular weight distribution of the lignin shows one major and 2 to 3 minor peaks with the maximum being under 3800. Purification of the crude lignin is most effectively done by redissolution in acetone and spray drying in vacuum at low temperature to avoid melting and resinification. A dried solid filter cake is easily broken up into a free flowing tan- colored powder.
  • the combined effect of high alcohol concentration and high pressure is an essential aspect of this invention in that it allows faster delignification of any wood species to low residual lignin content levels which earlier were not possible without considerable losses in cellulose viscosity.
  • the pressure effect diminishes somewhat when solvent compositions lower than 80:20 alcohol:water content are used.
  • Table 5 demonstrates the advantages of alcohol concentration higher than 80% by volume and overpressure on delignification and carbohydrate retention at a cooking temperature of 210°C.

Landscapes

  • Paper (AREA)

Claims (1)

  1. Procédé de digestion d'une matière lignocellulosique, en vue de recueillir de la cellulose fibreuse, par dissolution des parties constitutives lignine et hémicellulose de la matière lignocellulosique dans un alcool méthylique ou éthylique aqueux contenant, à l'état dissous, un chlorure ou un nitrate de magnésium, calcium ou baryum, ou du sulfate de magnésium, ou un mélange de ceux-ci, en quantité molaire de 0,001 à 1,0, pendant une durée n'excédant pas deux heures, à température élevée, supérieure à 130°C, et sous haute pression, la quantité de liqueur de cuisson étant d'au moins 4 parties en poids par partie pondérale de matière lignocellulosique, et récupération de la cellulose restée non dissoute, caractérisé par l'utilisation combinée des caractéristiques suivantes:
    1) la pression au cours de la cuisson est maintenue à une valeur supérieure d'au moins 5 bars à celle développée par les vapeurs de la liqueur de cuisson à la température de cuisson; et
    2) le méthanol ou éthanol aqueux contient entre 80 et 98 pour cent, en volume, de l'alcool.
EP19810902305 1980-07-25 1981-07-24 Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux Expired EP0056409B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81902305T ATE54190T1 (de) 1980-07-25 1981-07-24 Pulpen von lignocellulose mit waessrigem alkohol und einem alkali-erdmetallsalz-katalysator.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA359443 1980-07-25
CA000359443A CA1150012A (fr) 1980-07-25 1980-07-25 Preparation de la pate de lignocellulose en milieu aqueux par catalyse aux solvants

Publications (2)

Publication Number Publication Date
EP0056409A1 EP0056409A1 (fr) 1982-07-28
EP0056409B1 true EP0056409B1 (fr) 1990-06-27

Family

ID=4117790

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19810902305 Expired EP0056409B1 (fr) 1980-07-25 1981-07-24 Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux

Country Status (8)

Country Link
EP (1) EP0056409B1 (fr)
JP (1) JPH0329917B2 (fr)
BR (1) BR8108706A (fr)
CA (1) CA1150012A (fr)
DE (1) DE3177195D1 (fr)
FI (1) FI71781C (fr)
RU (1) RU1830091C (fr)
WO (1) WO1982000483A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AR227462A1 (es) * 1981-03-26 1982-10-29 Thermoform Bau Forschung Procedimiento mejorado para la produccion de hidrolizados de carbohidratos a partir de material celulosico triturado
US4699124A (en) * 1985-06-28 1987-10-13 Power Alcohol, Inc. Process for converting cellulose to glucose and other saccharides
EP0635080B1 (fr) * 1992-04-06 1997-03-12 A. Ahlstrom Corporation Procede de production de pate
WO2006067171A1 (fr) 2004-12-23 2006-06-29 Shell Internationale Research Maatschappij B.V. Procede d'hydrogenation d'une lactone ou d'un acide carboxylique ou d'un ester comprenant un groupe gamma-carbonyle
US20070034345A1 (en) * 2005-06-15 2007-02-15 Leonardus Petrus Process for organosolv pulping and use of a gamma lactone in a solvent for organosolv pulping
JP5136984B2 (ja) * 2007-04-04 2013-02-06 独立行政法人産業技術総合研究所 糖の製造方法
US8580978B2 (en) 2009-08-07 2013-11-12 Shell Oil Company Process for preparing a hydroxyacid or hydroxyester

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB416549A (en) * 1933-03-07 1934-09-07 Henry Dreyfus Improvements in the manufacture of cellulose and lignocellulosic materials
GB576785A (en) * 1942-03-11 1946-04-18 Henry Dreyfus Improvements in or relating to the manufacture of cellulose
CH386823A (de) * 1959-02-06 1965-01-15 Ceskoslovenska Akademie Ved Verfahren zur Gewinnung von nativem Lignin und Hemizellulose
CA1131415A (fr) * 1978-11-27 1982-09-14 Bau- Und Forschungsgesellschaft Thermoform A.G. Transformation en pate de la lignocellulose avec un melange aqueux d'un catalyseur et du methanol

Also Published As

Publication number Publication date
FI71781C (fi) 1987-02-09
DE3177195D1 (de) 1990-08-02
BR8108706A (pt) 1982-06-01
JPH0329917B2 (fr) 1991-04-25
WO1982000483A1 (fr) 1982-02-18
RU1830091C (ru) 1993-07-23
EP0056409A1 (fr) 1982-07-28
FI820927L (fi) 1982-03-17
JPS57501239A (fr) 1982-07-15
FI71781B (fi) 1986-10-31
CA1150012A (fr) 1983-07-19

Similar Documents

Publication Publication Date Title
SU1194282A3 (ru) Способ разложени лигноцеллюлозного материала
US4594130A (en) Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst
CA2091373C (fr) Procede de production des sucres anydres et sucres fermetissibles, a partir de liquides obtenus pyrolyse rapide
US7402224B1 (en) Method for producing paper pulp, lignins, sugars and acetic acid by frantionation of lignocellulosic vegetable material in formic/acetic acid medium
US4746401A (en) Process for extracting lignin from lignocellulosic material using an aqueous organic solvent and an acid neutralizing agent
Sarkanen Acid catalyzed delignification of lignocellulosics in organic solvents
EP2513150A1 (fr) Procédé pour l'extraction de sucres et de lignine à partir de biomasse solide comprenant de la lignocellulose
JPS62111700A (ja) リグノセルロ−ス植物性原料からグルコ−ス、リグニンおよびセルロ−スを回収する方法
CZ20013627A3 (cs) Způsob dělení biomasy obsahující lignocelulózu
Guo et al. Efficient separation of functional xylooligosaccharide, cellulose and lignin from poplar via thermal acetic acid/sodium acetate hydrolysis and subsequent kraft pulping
Ibrahim et al. Prehydrolysis and organosolv delignification process for the recovery of hemicellulose and lignin from beech wood
EP0056409B1 (fr) Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux
US2686120A (en) Alkaline pulping of lignocellulose in the presence of oxygen to produce pulp, vanillin, and other oxidation products of lignin substance
US2673148A (en) Alkaline pulping using gaseous oxygen
Miranda et al. Kinetics of ASAM and kraft pulping of eucalypt wood (Eucalyptus globulus)
US11624152B2 (en) Low energy production process for producing paper pulp from lignocellulosic biomass
JPS6328157B2 (fr)
Faass et al. Buffered solvent pulping
EP0074983B1 (fr) Procede de saccharification a haut rendement par un solvant organique
US2772968A (en) Process of pulping cellulosic materials with triethylene glycol
NO832783L (no) Fremgangsmaate for delignifisering av ved og andre lignocelluloseholdige produkter
US1581671A (en) Production of pulp and other products from wood
EP4261343A1 (fr) Conversion de résidus de biomasse en bio-huile
US20210139653A1 (en) Process for the production of bioproducts from lignocellulosic material
RU2763878C1 (ru) Способ получения целлюлозы для химической переработки из целлюлозосодержащего сырья

Legal Events

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

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): AT DE FR SE

17P Request for examination filed

Effective date: 19820806

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT DE FR SE

REF Corresponds to:

Ref document number: 54190

Country of ref document: AT

Date of ref document: 19900715

Kind code of ref document: T

REF Corresponds to:

Ref document number: 3177195

Country of ref document: DE

Date of ref document: 19900802

ET Fr: translation filed
R20 Corrections of a patent specification

Effective date: 19900912

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19940131

Year of fee payment: 13

EAL Se: european patent in force in sweden

Ref document number: 81902305.2

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Effective date: 19950401

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19990728

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 19990729

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 19990730

Year of fee payment: 19

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000724

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000725

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20000731

EUG Se: european patent has lapsed

Ref document number: 81902305.2

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

APAH Appeal reference modified

Free format text: ORIGINAL CODE: EPIDOSCREFNO