WO1982000483A1 - 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

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Publication number
WO1982000483A1
WO1982000483A1 PCT/EP1981/000105 EP8100105W WO8200483A1 WO 1982000483 A1 WO1982000483 A1 WO 1982000483A1 EP 8100105 W EP8100105 W EP 8100105W WO 8200483 A1 WO8200483 A1 WO 8200483A1
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WO
WIPO (PCT)
Prior art keywords
acid
cooking
cooking liquor
alcohol
zero
Prior art date
Application number
PCT/EP1981/000105
Other languages
English (en)
Inventor
Bau Forschungs Thermoform
L Paszner
P Chang
Original Assignee
Thermoform Bau Forschung
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 Thermoform Bau Forschung filed Critical Thermoform Bau Forschung
Priority to AT81902305T priority Critical patent/ATE54190T1/de
Priority to DE8181902305T priority patent/DE3177195D1/de
Priority to BR8108706A priority patent/BR8108706A/pt
Publication of WO1982000483A1 publication Critical patent/WO1982000483A1/fr
Priority to FI820927A priority patent/FI71781C/fi
Priority to SU823411783A priority patent/RU1830091C/ru

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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 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.

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  • 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.
PCT/EP1981/000105 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 WO1982000483A1 (fr)

Priority Applications (5)

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.
DE8181902305T DE3177195D1 (de) 1980-07-25 1981-07-24 Pulpen von lignocellulose mit waessrigem alkohol und einem alkali-erdmetallsalz-katalysator.
BR8108706A BR8108706A (pt) 1980-07-25 1981-07-24 Polpacao de lignocelulose com alcool aquoso e catalisador de sal de metal alcalino terroso
FI820927A FI71781C (fi) 1980-07-25 1982-03-17 Kokning av lignocellulosa med vattenhaltig alkohol och jordalkalimetallsaltkatalysator.
SU823411783A RU1830091C (ru) 1980-07-25 1982-03-24 Способ варки лигноцеллюлозного материала

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA000359443A CA1150012A (fr) 1980-07-25 1980-07-25 Preparation de la pate de lignocellulose en milieu aqueux par catalyse aux solvants
CA359443800725 1980-07-25

Publications (1)

Publication Number Publication Date
WO1982000483A1 true WO1982000483A1 (fr) 1982-02-18

Family

ID=4117790

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1981/000105 WO1982000483A1 (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)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982003409A1 (fr) * 1981-03-26 1982-10-14 Bau Forschung Thermoform Procede de saccharification a haut rendement par un solvant organique
WO1993020279A1 (fr) * 1992-04-06 1993-10-14 A. Ahlstrom Corporation Procede de production de pate
WO2006134126A1 (fr) * 2005-06-15 2006-12-21 Shell Internationale Research Maatschappij B.V. Procede pour une pulpation organosolv et utilisation de gamma lactone dans un solvant destine a une pulpation organosolv
US8003818B2 (en) 2004-12-23 2011-08-23 Shell Oil Company Process for the hydrogenation of a lactone or of a carboxylic acid or an ester having a gamma-carbonyl group
US8580978B2 (en) 2009-08-07 2013-11-12 Shell Oil Company Process for preparing a hydroxyacid or hydroxyester

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4699124A (en) * 1985-06-28 1987-10-13 Power Alcohol, Inc. Process for converting cellulose to glucose and other saccharides
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2022654A (en) * 1933-03-07 1935-12-03 Dreyfus Henry Treatment of cellulosic materials
US2560638A (en) * 1942-03-11 1951-07-17 Celanese Corp Manufacture of cellulose
CH386823A (de) * 1959-02-06 1965-01-15 Ceskoslovenska Akademie Ved Verfahren zur Gewinnung von nativem Lignin und Hemizellulose
DE2920731A1 (de) * 1978-11-27 1980-05-29 Thermoform Bau Forschung Verfahren zur chemischen umwandlung von lignocellulose unter abtrennung von fasern davon

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2022654A (en) * 1933-03-07 1935-12-03 Dreyfus Henry Treatment of cellulosic materials
US2560638A (en) * 1942-03-11 1951-07-17 Celanese Corp Manufacture of cellulose
CH386823A (de) * 1959-02-06 1965-01-15 Ceskoslovenska Akademie Ved Verfahren zur Gewinnung von nativem Lignin und Hemizellulose
DE2920731A1 (de) * 1978-11-27 1980-05-29 Thermoform Bau Forschung Verfahren zur chemischen umwandlung von lignocellulose unter abtrennung von fasern davon

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982003409A1 (fr) * 1981-03-26 1982-10-14 Bau Forschung Thermoform Procede de saccharification a haut rendement par un solvant organique
WO1993020279A1 (fr) * 1992-04-06 1993-10-14 A. Ahlstrom Corporation Procede de production de pate
US8003818B2 (en) 2004-12-23 2011-08-23 Shell Oil Company Process for the hydrogenation of a lactone or of a carboxylic acid or an ester having a gamma-carbonyl group
WO2006134126A1 (fr) * 2005-06-15 2006-12-21 Shell Internationale Research Maatschappij B.V. Procede pour une pulpation organosolv et utilisation de gamma lactone dans un solvant destine a une pulpation organosolv
US8580978B2 (en) 2009-08-07 2013-11-12 Shell Oil Company Process for preparing a hydroxyacid or hydroxyester

Also Published As

Publication number Publication date
FI71781C (fi) 1987-02-09
BR8108706A (pt) 1982-06-01
CA1150012A (fr) 1983-07-19
EP0056409B1 (fr) 1990-06-27
JPH0329917B2 (fr) 1991-04-25
FI820927L (fi) 1982-03-17
DE3177195D1 (de) 1990-08-02
JPS57501239A (fr) 1982-07-15
EP0056409A1 (fr) 1982-07-28
FI71781B (fi) 1986-10-31
RU1830091C (ru) 1993-07-23

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