EP0056409A1 - 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.

Info

Publication number
EP0056409A1
EP0056409A1 EP19810902305 EP81902305A EP0056409A1 EP 0056409 A1 EP0056409 A1 EP 0056409A1 EP 19810902305 EP19810902305 EP 19810902305 EP 81902305 A EP81902305 A EP 81902305A EP 0056409 A1 EP0056409 A1 EP 0056409A1
Authority
EP
European Patent Office
Prior art keywords
acid
cooking
cooking liquor
zero
alcohol
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
EP19810902305
Other languages
German (de)
English (en)
Other versions
EP0056409B1 (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

    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/20Pulping cellulose-containing materials with organic solvents or in solvent environment

Definitions

  • the invention relates to a method for the digestion of lignocellulose material which comprises cooking the fragmented lignocellulose material with an aqueous methyl or ethyl alcohol containing dissolved therein an alkaline earth metal salt, namely a chloride or nitrate of magnesium, calcium or barium or magnesium sulfate or a soluble mixture thereof in a concentration of less than 1.0 molar and, optionally, an acid reacting substance in a concentration of Less than 0.008 normal for not more than two hours at a temperature above 130°C, the amount of cooking liquor being at least 4 parts by weight per part by weight of the lignocellulose material, recovering the fibres liberated thereby from the cooking liquor, and separating the remaining spent cooking liquor into solvent, lignin and sugars.
  • an alkaline earth metal salt namely a chloride or nitrate of magnesium, calcium or barium or magnesium sulfate or a soluble mixture thereof in a concentration of less than 1.0 molar and, optional
  • the problem to be solved by the invention is to improve deligniflcation 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.
  • Great Britain patent No. 357 821 (Kleinert) describes a process for the decomposition of vegetable fibrous matter for the purpose of obtaining the cellulose and the incrusting materials which uses as the decomposing agent mixtures of alcohol and water with a water content of 20 to 75 percent by weight and states on page 1, lines 74 to 77, that with 96 percent alcohol a dark brown residue amounting to 92 percent of the raw material is obtained.
  • angewandte Chemie 44 (1931), pages 788 to 791, states on page 789 that absolute alcohol solves only little lignin and nearly no carbohydrates, and on same page, lines 4 to 2 from the bottom with reference to figure 1 that maximum digestion results with an alcohol content of 45 to 50 percent, and United States patent No. 3 585 104 (Kleinert) states in lines 42 to 44 of c.2 that methanol or ethanol in the medium concentration range between about 20 per cent and 75 percent by weight alcohol content have a stronger delignifying effect upon fibrous plant materials than the water-free alcohols.
  • methanol is the preferred alcohol, bute where methanol is not available in sufficient amount ethanol can be used as well.
  • the preferred alcohol content of the cooking liquor is 80 to 98 pe rc e n t 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.
  • 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 process also appeals to be quite tolerant to extended cooking times wherein the parameter most affected is residual lignin content.
  • 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 percent 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 lingin 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.

Landscapes

  • Paper (AREA)

Abstract

Un rendement eleve en pate de haute qualite est obtenu par cuisson d'un materiau de lignocellulose fragmente a une temperature comprise entre 180 et240oc avec un melange de methanol ou d'ethanol et d'eau contenant 80 a 98% en volume d'alcool, le melange contenant entre 0,001 et 0,5 mole d'un sel de metal alcalino-terreux dissout, et de zero a 0,005 normal/mole de (a) un acide mineral fort, ou (b) un acide mineral faible ou (c) un acide organique faible ou (d) un sel d'un metal reagissant a l'acide pour favoriser la delignification rapide. De plus, on peut utiliser des pressions sensiblement plus elevees que celles developpees dans les espaces fermes par les vapeurs du melange solvant a la temperature de cuisson pour encore davantage la vitesse de delignification et supprimer la degradation de l'hydrate de carbone. La lignine est obtenue sous forme de poudre par evaporation a basse temperature de l'alcool de la liqueur de cuisson utilisee.
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 true EP0056409A1 (fr) 1982-07-28
EP0056409B1 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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO8200483A1 *

Also Published As

Publication number Publication date
FI71781C (fi) 1987-02-09
DE3177195D1 (de) 1990-08-02
BR8108706A (pt) 1982-06-01
EP0056409B1 (fr) 1990-06-27
JPH0329917B2 (fr) 1991-04-25
WO1982000483A1 (fr) 1982-02-18
RU1830091C (ru) 1993-07-23
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
US4594130A (en) Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst
SU1194282A3 (ru) Способ разложени лигноцеллюлозного материала
CA2091373C (fr) Procede de production des sucres anydres et sucres fermetissibles, a partir de liquides obtenus pyrolyse rapide
US4746401A (en) Process for extracting lignin from lignocellulosic material using an aqueous organic solvent and an acid neutralizing agent
EP0043342B1 (fr) Méthode pour la délignification du bois et autres produits ligno-cellulosiques
RU2534067C2 (ru) Способ получения целлюлозы из биомассы, содержащей лигноцеллюлозу
JP3348387B2 (ja) ギ酸を添加した酢酸によるパルプの製法
US20140073016A1 (en) Treatment
GB1582480A (en) Process for the production of glucose
RU2682348C2 (ru) Способ экстракции лигнина
US2673148A (en) Alkaline pulping using gaseous oxygen
DE10297032T5 (de) Verfahren zur Zellstoffherstellung
EP0056409A1 (fr) Production de pate de lignocellulose avec de l'alcool aqueux et un catalyseur d'un sel d'un metal alcalino-terreux.
CA1131415A (fr) Transformation en pate de la lignocellulose avec un melange aqueux d'un catalyseur et du methanol
US2772968A (en) Process of pulping cellulosic materials with triethylene glycol
NO832783L (no) Fremgangsmaate for delignifisering av ved og andre lignocelluloseholdige produkter
US1902916A (en) Process for decomposing plant fiber material by cooking with phenolates
DD147259A5 (de) Verfahren zur chemischen umwandlung von lignocellulose
US11118017B2 (en) Process for the production of bioproducts from lignocellulosic material
CA1057008A (fr) Methode de fabrication de pates au sulfite
Nada et al. Influence of surrounding gases on soda-anthraquinone pulping of cotton stalks
CA1229334A (fr) Fractionnement de la biomasse
US4235666A (en) 1,2,3,4,4a,9a-Hexahydro-9,10-anthracene-dione, its preparation and its application to the delignification of lignocellulosic materials
Trembus et al. USED PULPING LIQUORS APPLICATION IN ОXIDATIVE–ORGANOSOLVENT TECHNOLOGY OF STRAW CELLULOSE PRODUCTION
NL8200241A (nl) Werkwijze voor het ontsluiten van ligno-cellulose-materiaal.

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