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WO2004029356A1 - Procede permettant d'obtenir une fraction - Google Patents

Procede permettant d'obtenir une fraction Download PDF

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Publication number
WO2004029356A1
WO2004029356A1 PCT/SE2003/001478 SE0301478W WO2004029356A1 WO 2004029356 A1 WO2004029356 A1 WO 2004029356A1 SE 0301478 W SE0301478 W SE 0301478W WO 2004029356 A1 WO2004029356 A1 WO 2004029356A1
Authority
WO
WIPO (PCT)
Prior art keywords
pulping
fraction
low molecular
soda
liquor
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.)
Ceased
Application number
PCT/SE2003/001478
Other languages
English (en)
Inventor
Eva Lisa Lindfors
Fredrik Berthold
Hans Theliander
Leelo Olm
Per Tomani
Peter AXEGÅRD
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.)
STFI Skogsindustrins Tekniska Forskningsinstitut AB
Original Assignee
STFI Skogsindustrins Tekniska Forskningsinstitut AB
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 STFI Skogsindustrins Tekniska Forskningsinstitut AB filed Critical STFI Skogsindustrins Tekniska Forskningsinstitut AB
Priority to AU2003263714A priority Critical patent/AU2003263714A1/en
Publication of WO2004029356A1 publication Critical patent/WO2004029356A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • 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
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes

Definitions

  • This invention concerns the technical field of alkaline pulping processes, e.g sulfate pulping, soda pulping and alkaline sulfite pulping processes, in particular it relates to the separation of a low molecular fraction from a liquor obtained by alkaline treatment of organic material, e.g. wood, annual fibres and plant waste material such as citrus and apple waste and sugar beet waste, useful for enhancing the cooking results and a method for obtaining that fraction. Further, the low molecular fraction enables increased delignif ⁇ cation, brighter pulp and improved bleachability. Further the invention relates to the separation of a high molecular fraction for use as e.g. fuel raw material or as chemical feed stock for the chemical industry.
  • organic material e.g. wood, annual fibres and plant waste material such as citrus and apple waste and sugar beet waste
  • the present invention solves one or more of the above problems by providing according to a first aspect a method for obtaining a low molecular black liquor fraction comprising the following steps: a) separating black liquor into two fractions by using separation means with a cut off of approximately 100 kDa or smaller, or by adding a salt preferably a calcium salt, enabling coagulation; and b) recovering the low molecular fraction.
  • the present invention also provides according to a second aspect a method according to the first aspect comprising a further step: recovery of the high molecular fraction which is useful as a fuel raw material which easily may be transported away e.g. in the form of pellets or powder or any other suitable form, from the pulping site and used as fuel raw material in another site e.g.
  • the present invention thus enables recycling of black liquor components, at the same enabling extracting high molecular components, > 1000 Da, suitable for use as fuel raw material.
  • the fractionation procedure also results in removal of divalent cations, e.g. Ca 2+ , from the low molecular weight fraction while the inorganic species active in cooking, e.g. OH " and SH " will be found in the low molecular weight fraction.
  • the present invention also provides according to a third aspect a low molecular black liquor fraction obtainable by a method according to the first aspect.
  • the present invention also provides according to a fourth aspect a composition for enhancing the production of chemical pulp based on alkaline processes, e.g.
  • sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes comprising a substance/substances of carbohydratic origin or a low molecular black liquor fraction according to the third aspect.
  • the present invention also provides according to a fifth aspect a method for enhancing the production of chemical pulp based on alkaline processes, e.g. sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes comprising adding a composition according to the fourth aspect or a low molecular black liquor fraction according to the third aspect.
  • the present invention also provides according to a sixth aspect use of a composition according to the fourth aspect or a low molecular black liquor fraction according to the third aspect in alkaline pulping processes, e.g. sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes, e.g. by adding a composition according to the fourth aspect into a cooking liquor or using said composition as a cooking liquor self.
  • alkaline pulping processes e.g. sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes
  • pectin or pectic substances refer to the family of polysaccharides extractable from plant material using e.g. hot water, ammonium oxalate, weak acid or chelating reagents and alkali, characterized by the presence of methyl esterified and/or non-methyl esterified galactouronic acid, including type I rhamnogalactouronan(s), type II rhamnogalactouronan(s), xylogalactouronan(s) and homogalactouronan(s).
  • drying liquor embrace any liquor, solution, dispersion or similar mixture, e.g. white liquor, that will be usable in the industrial production of chemical pulp based on alkaline processes, e.g. sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes, that those skilled in the art to which the invention pertains would use in the production of chemical pulp based on alkaline processes.
  • black liquor embrace any liquor, solution, dispersion or similar obtainable from alkaline treatment of organic material.
  • This organic material may be wood, fruit, annual plants or vegetables or material derivable from said materials.
  • the black liquor is present in a mill for use in the manufacture of pulp and/or paper.
  • low molecular black liquor fraction or “low molecular fraction” or “low molecular dialysate” (used interchangeably in the present description) embrace any fraction obtainable from black liquor with a molecular weight less than approximately 100 000 Da (lOOkDa) or smaller. This fraction contain material dissolved from the wood raw material both in their native form and and forms altered under the process.
  • the low molecular weight fraction also comprises pectin or one or more compounds related to or derivable from pectin or a pectic substance.
  • the low molecular fraction may be in liquid phase or in a solid phase.
  • high molecular fraction or “high molecular residue” (used interchangeably in the present description) embrace any fraction obtainable from black liquor that in the most general case have a molecular weight above approximately 100000 Da and more particularly a molecular weight above 1000 Da.
  • the high molecular fraction normally comprises a lot of lignin and multivalent ions
  • the separation in step a) is performed using separation means with a cut off of 10 kDa, preferably separation means with a cut off of 1 kDa.
  • the method comprises a further step c): treatment of the low molecular fraction obtained during step b) with an acidic liquid, preferably concentrated hydrochloric acid, rendering into a pH of from approximately 1 to 7, . ' preferably approximately pH 5, and the precipitation of a solid material, and removal of the precipitate, and recovering the liquid phase containing a low molecular fraction.
  • an acidic liquid preferably concentrated hydrochloric acid
  • an in water non-soluble solvent preferably ethyl acetate
  • ethyl acetate ethyl acetate
  • evaporating preferably by using a rotary vaporator, excess solvent from the organic layer
  • the method comprises a further step d): i) optionally the reduction of volume of the low molecular fraction obtained during step b) or step c), preferably by evaporation to half volume of the low molecular fraction obtained during step b) or step c), ii) precipitation using ethanol, methanol or isopropanol or any other suitable solvent in such proportions so that precipitation occurs, preferably in an amount of 1:1 (volume: volume), preferably using ethanol 1:1 (volume:volume), and iii) re-dissolution of said precipitate containing the low molecular fraction in water or other suitable solution (for cooking of pulp) e.g. white liquor, preferably water.
  • the low molecular fraction is now a light yellowish powder which produces a yellow-brown solution in water. It darkens on standing
  • the separation means with a cut off of 100 kDa , the separation means with a cut off of 10 kDa and the separation means with a cut off of I kDa is a dialysis equipment or a cross flow filter apparatus.
  • the high molecular fraction is formed to an easily movable form of fuel raw material, preferably powder or pellets, preferably by using drying or, if stored at elevated temperature, a pumpable liquor.
  • the fuel raw material may be sulfur depleted or otherwise pretreated in order to be used as a fuel.
  • the substance/substances of carbohydratic origin is (are) a polysaccharide(s) or one or more fractions thereof.
  • the polysaccharide(s) is (are) derived from pectin or a pectic compound, preferably a methyl esterified and/or non-methyl esterified galactouronic acid, including type I rhamnogalactouronanes, type II rhamnogalactouronanes, xylogalactouronan and homogalactouronan. or a combination thereof.
  • the pectin derived compound may further be degraded pectin or degraded forms of methyl esterified and/or non-methyl esterified galactouronic acid, including type I rhamnogalactouronanes, type II rhamnogalactouronanes, xylogalactouronan and homogalactouronan.
  • the composition is adjusted to contain the necessary ion concentrations which are suitable for the process, i.e. sulfate pulping including polysulfide pulping, soda-aq pulping, soda pulping and alkaline sulfite processes, preferably sulfate cooking, whereby preferably the composition may be adjusted to a OH ' -concentration of approximately 0.4 M, a SH " -concentration of approximately 0.22 M and a Na + -concentration of approximately 2.4 M if the water-wood material ratio is 20 : 1 (liquid : wood).
  • the person skilled in the art may adjust the above ion concentrations to fit a suitable water-wood material ratio so that the composition fulfils the definition cooking liquor.
  • a cooking liquor comprising a composition according the fourth aspect of the present invention.
  • the active compound or fraction is present in an amount of 0.001 % -100 % (weight/weight; when regarding the weight of the wood raw material) or in liquor-to-wood ratios between 3 to 50 : 1, preferably 3 to 8:1, (when referring to the amount of a liquid fraction added in relation to weight of the raw material), preferably in an amount of 0.001 % -20 % if in solid form, e.g. in the form of a powder (weight/weight; when regarding the weight of the wood raw material).
  • the composition according to the fourth aspect is used for the preparation of a cooking liquor.
  • the method according to the first aspect of the present invention thus provide for improved utilization of black liquors based on fractionation.
  • the low molecular fraction obtainable by the method according to the first aspect further achieves that a retained or an enhanced delignifing effect is achieved.
  • the pulp becomes brighter and thus is much more easy to bleach.
  • a removal of Ca 2+ or Mn 2+ ions, or other multivalent ions may be desired, which is achieved simultaneously when the high molecular fraction is removed from the black liquor as the multivalent ions normally adhere to lignins.
  • Preferred features of each aspect of the invention are as for each of the other aspects mutatis mutandis.
  • Fig 1 shows the effect of addition of black liquor (and fractions thereof) on delignificationrate.
  • Fig 2 shows fractionation of black liquor.
  • a kraft cooking liquor was adjusted so that the OH " concentration was 0.4 M, the SH " concentration 0.22 M and the Na + concentration 2.4 M.
  • the temperature was raised from 145 °C with a rate of approximately 2 °C/min and kept at 170 °C. Total time including raise to temperature was 100 min in stage two. After drainage of the cooking liquor the pulp was treated in a disintegrator and carefully washed before analysis.
  • a kraft black liquor was dialyzed using a membrane with molecular weight cut off of 1000.
  • The'dialysate liquor was adjusted to the same OH " and Na + concentration as the black liquor. This produced a low molecular weight dialysate (Dl) and a high molecular weight residue.
  • a cooking liquor based on the black liquor dialysate Dl was adjusted so that the OH " concentration was 0.4 M (using standard methods for black liquors), the SH " concentration 0.22 M and the Na + concentration 2.4 M.
  • a new liquor (D2) was produced from the dialysate liquor Dl by acidification using concentrated hydrochloric acid to a pH of 7 and the precipitate removed.
  • a cooking liquor based on the liquor fraction D2 was adjusted so that the OH " concentration was 0.4 M (using standard methods for black liquors), the SH " concentration 0.22 M and the Na + concentration 2.4 M.
  • a new liquor (D3) was produced from the liquor D2 by acidification using concentrated hydrochloric acid to a pH of 5.
  • the D3 fraction was washed using ethyl acetate and subsequently put on a rotary vaporator to remove residual ethyl acetate.
  • a cooking liquor based on the liquor fraction D3 was adjusted so that the OH " concentration was 0.4 M (using standard methods for black liquors), the SH " concentration 0.22 M and the Na + concentration 2.4 M.
  • To 4 g o.d. spruce wood chips, soaked in water over night and placed in a steel digester 80 ml of said liquor was added and the digester was immersed in a glycol bath at 70 °C. After this the same general procedure as in example 1 was followed.
  • a new liquor (D4) was produced from the liquor D3 by: 1) evaporation to half original volume 2) precipitation using ethanol 1 : 1 v:v 3) re-dissolution of said precipitate in water.
  • a cooking liquor based on the fraction D4 was adjusted so that the OH " concentration was 0.4 M (using standard methods for black liquors), the SH " concentration 0.22 M and the Na + concentration 2.4 M.
  • Table 1 The results from the above examples are summarized in table 1 below and they are also depicted in figure 2.

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  • Paper (AREA)

Abstract

La présente invention concerne un procédé permettant d'obtenir une fraction de liqueur résiduaire à faible poids moléculaire. Ce procédé comporte les étapes suivantes : a) séparation de la liqueur résiduaire en deux fractions à l'aide d'un moyen de séparation ayant une coupe d'environ 100 kDa maximum, ou par addition d'un sel, de préférence, d'un sel de calcium, permettant la coagulation; et b) l'extraction de la fraction à faible poids moléculaire. La présente invention concerne également un procédé comportant une autre étape: récupération de la fraction à haut poids moléculaire utile comme une source de combustible qui peut facilement être éloignée de ce site pour être utilisée sur un autre site. La présente invention concerne une fraction de liqueur résiduaire à faible poids moléculaire obtenue par le procédé susmentionné. La présente invention concerne également une composition permettant d'améliorer la production de pâte chimique sur la base de procédés alcalins, par exemple, la procédé kraft alcalin, y comprise la cuisson au polysulfure, la cuisson à la soude AQ, la cuisson à la soude et la cuisson au bisulfite alcalin comprenant une substance/des substances d'origine hydrate de carbone ou une fraction de liqueur résiduaire de faible poids moléculaire. La présente invention concerne également un procédé permettant d'améliorer la production de pâte chimique sur la base de procédés alcalins, par exemple, le procédé kraft alcalin, y compris la cuisson au polysulfure, la cuisson à la soude AQ, la cuisson à la soude et la cuisson au bisulfite alcalin comportant l'addition d'une composition ou fraction de liqueur résiduaire de faible poids moléculaire. La présente invention concerne l'utilisation d'une composition ou une fraction de liqueur résiduaire de faible poids moléculaire dans les procédés kraft alcalin, par exemple, les procédés de pâte au sulfate, y compris la cuisson au polysulfure, la cuisson à la soude AQ, la cuisson à la soude et la cuisson au bisulfite alcalin.
PCT/SE2003/001478 2002-09-27 2003-09-23 Procede permettant d'obtenir une fraction Ceased WO2004029356A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003263714A AU2003263714A1 (en) 2002-09-27 2003-09-23 Method for obtaining a fraction

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE0202869-4 2002-09-27
SE0202869A SE0202869D0 (sv) 2002-09-27 2002-09-27 Method for obtaining a fraction

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WO2004029356A1 true WO2004029356A1 (fr) 2004-04-08

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007120091A1 (fr) * 2006-03-16 2007-10-25 Stfi-Packforsk Ab Procédé permettant de séparer du pentose polymérique d'un liquide/d'une suspension épaisse
EP2044184A4 (fr) * 2006-07-11 2011-03-23 Pioneer Biofuel Inc Production d'un produit d'alimentation de raffinerie à partir de savons produits durant un procédé de fabrication de pâtes chimiques
CN107207628A (zh) * 2015-01-26 2017-09-26 日本制纸株式会社 含有木聚糖的物质的制造方法
EP3116937A4 (fr) * 2014-03-12 2018-02-07 Ren Fuel K2B AB Procédé pour une extraction efficace de la lignine
US9982004B2 (en) 2012-08-24 2018-05-29 Upm-Kymmene Corporation Method for recovering low molecular weight lignin from a filtrate

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4728393A (en) * 1985-11-20 1988-03-01 Domtar Inc. Methods for obtaining deicers from black liquor
US4764596A (en) * 1985-11-05 1988-08-16 Repap Technologies Inc. Recovery of lignin
US4966650A (en) * 1987-09-17 1990-10-30 Delong Edward A Method for fractionation of lignins from steam exploded lignocellulosics to provide fractions with different properties
US6103059A (en) * 1993-06-16 2000-08-15 Lignozym Gmbh Process for delignification of a lignin containing pulp

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4764596A (en) * 1985-11-05 1988-08-16 Repap Technologies Inc. Recovery of lignin
US4728393A (en) * 1985-11-20 1988-03-01 Domtar Inc. Methods for obtaining deicers from black liquor
US4966650A (en) * 1987-09-17 1990-10-30 Delong Edward A Method for fractionation of lignins from steam exploded lignocellulosics to provide fractions with different properties
US6103059A (en) * 1993-06-16 2000-08-15 Lignozym Gmbh Process for delignification of a lignin containing pulp

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007120091A1 (fr) * 2006-03-16 2007-10-25 Stfi-Packforsk Ab Procédé permettant de séparer du pentose polymérique d'un liquide/d'une suspension épaisse
EP2044184A4 (fr) * 2006-07-11 2011-03-23 Pioneer Biofuel Inc Production d'un produit d'alimentation de raffinerie à partir de savons produits durant un procédé de fabrication de pâtes chimiques
CN101506340B (zh) * 2006-07-11 2012-06-13 布卢基能源股份有限公司 从化学制浆过程期间产生的皂生产精炼料
US9982004B2 (en) 2012-08-24 2018-05-29 Upm-Kymmene Corporation Method for recovering low molecular weight lignin from a filtrate
EP3116937A4 (fr) * 2014-03-12 2018-02-07 Ren Fuel K2B AB Procédé pour une extraction efficace de la lignine
CN107207628A (zh) * 2015-01-26 2017-09-26 日本制纸株式会社 含有木聚糖的物质的制造方法
EP3252083A4 (fr) * 2015-01-26 2018-09-05 Nippon Paper Industries Co., Ltd. Procédé de fabrication d'un matériau contenant du xylane
US10316108B2 (en) 2015-01-26 2019-06-11 Nippon Paper Industries Co., Ltd. Method for producing xylan-containing material
CN107207628B (zh) * 2015-01-26 2020-02-21 日本制纸株式会社 含有木聚糖的物质的制造方法

Also Published As

Publication number Publication date
AU2003263714A1 (en) 2004-04-19
SE0202869D0 (sv) 2002-09-27

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