EP0056409B1 - Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst - Google Patents

Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst Download PDF

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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)
French (fr)
Other versions
EP0056409A1 (en
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/en
Application granted granted Critical
Publication of EP0056409B1 publication Critical patent/EP0056409B1/en
Expired legal-status Critical Current

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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 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)
EP19810902305 1980-07-25 1981-07-24 Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst Expired EP0056409B1 (en)

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
CA000359443A CA1150012A (en) 1980-07-25 1980-07-25 Aqueous catalysed solvent pulping of lignocellulose
CA359443 1980-07-25

Publications (2)

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

Family

ID=4117790

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19810902305 Expired EP0056409B1 (en) 1980-07-25 1981-07-24 Pulping of lignocellulose with aqueous alcohol and alkaline earth metal salt catalyst

Country Status (8)

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

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
WO1993020279A1 (en) * 1992-04-06 1993-10-14 A. Ahlstrom Corporation Method of producing pulp
BRPI0519615A2 (pt) 2004-12-23 2009-02-25 Shell Int Research processo para a hidrogenaÇço de um reagente, e, composiÇço combustÍvel
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
GB416416A (en) * 1933-03-07 1934-09-07 Henry Dreyfus Improvements in the manufacture of cellulose from ligno-cellulosic 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 (en) * 1978-11-27 1982-09-14 Bau- Und Forschungsgesellschaft Thermoform A.G. Pulping of lignocellulose with aqueous methanol/ catalyst mixture

Also Published As

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

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