EP1753908B1 - Verfahren zur herstellung eines chemiezellstoffes - Google Patents

Verfahren zur herstellung eines chemiezellstoffes Download PDF

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Publication number
EP1753908B1
EP1753908B1 EP05741840.2A EP05741840A EP1753908B1 EP 1753908 B1 EP1753908 B1 EP 1753908B1 EP 05741840 A EP05741840 A EP 05741840A EP 1753908 B1 EP1753908 B1 EP 1753908B1
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EP
European Patent Office
Prior art keywords
pulp
weight
cellulose
lye
content
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EP05741840.2A
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German (de)
English (en)
French (fr)
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EP1753908A1 (de
Inventor
Herbert Sixta
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
    • 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
    • D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for
    • 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
    • D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
    • D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor

Definitions

  • the present invention relates to a process for producing a chemical pulp according to the preamble of claim 1.
  • the production of chemical pulps is dominated by the acidic bisulfite digestion process as well as the prehydrolysis force process.
  • the acidic bisulfite digestion process is a very environmentally friendly technology due to the high yield and the good opportunities to utilize by-products and waste products or to use for energy.
  • the known purification steps involve both the removal of non-cellulosic material, e.g. Extracts, lignins and hemicelluloses, as well as the change in molecular weight distribution towards a close, monomodal distribution with a minimum of low molecular weight carbohydrates.
  • alkali extraction is usually used.
  • the pulp is treated with alkali and then squeezed.
  • cold alkaline extraction CCE
  • hot alkali extraction HCE
  • CCE cold alkaline extraction
  • hot alkali extraction HCE
  • the cold alkaline extraction which is usually carried out at temperatures just above room temperature, causes essentially physical changes in the pulp
  • hot alkali extraction at typical temperatures of 70 ° C to 120 ° C causes a variety of chemical reactions.
  • the use of cold alkaline extraction encounters great difficulties in practice, since very high amounts of alkali are needed.
  • At 10% by weight pulp consistency and a concentration of 10% NaOH it is necessary to use about 1 ton of NaOH per ton of pulp.
  • the object of the present invention is to provide an improved process for the production of chemical pulps, in which the above-described disadvantages in carrying out a cold and / or hot alkali extraction step can be avoided.
  • beta-cellulose By the term “beta-cellulose”, one skilled in the art will understand that proportion in a cellulosic material which (unlike alpha-cellulose) is soluble in a 17.5% solution of NaOH at 20 ° C, but on acidification of the solution (as opposed to gamma-cellulose) precipitates again with 4.75M H 2 SO 4 .
  • At least a portion of the recirculated liquor is treated by means of a membrane separation process.
  • the membrane separation process is preferably a nano or an ultrafiltration process.
  • membranes having a cut-off of ⁇ 2000 g / mol, in particular ⁇ 1000 g / mol, for carrying out nanofiltration preference is given to using membranes having a cut-off of ⁇ 2000 g / mol, in particular ⁇ 1000 g / mol, for carrying out nanofiltration.
  • 100% of the beta-cellulose and more than 50% of the gamma-cellulose, preferably more than 70% can be removed.
  • the ratio between retentate and permeate is set between 2 and 5, preferably between 4 and 5.
  • 100% of the beta-cellulose and more than 10% of the gamma-cellulose, preferably more than 30% can be removed.
  • the ratio between retentate and permeate is set between 2 and 5, preferably between 4 and 5.
  • the permeate from the membrane separation process can be supplied wholly or partly to the leach tank, from which the liquor used to treat the pulp is taken.
  • beta-cellulose Another way to reduce the content of beta-cellulose is that at least a portion of the recirculated liquor is thermally treated. In this case, that part of the beta-cellulose, which (such as xylan) has no branched structures, degraded to gamma-cellulose.
  • the thermal treatment is preferably carried out at a temperature of more than 50 ° C, preferably more than 70 ° C, for a period of 10 minutes to 300 minutes, preferably 30 minutes.
  • the pressing liquor is treated both by means of a membrane separation process as well as thermally.
  • the pressing liquor can be pre-cleaned by means of a filter to remove undissolved particles.
  • a preferred embodiment of the process according to the invention is characterized in that the extraction step is a cold alkali extraction in which the treatment of the pulp with caustic is carried out at a temperature of less than 50 ° C, preferably less than 25 ° C.
  • the treatment of the pulp with lye is preferred at a pulp density of more than 5 wt.%, Preferably 10 wt.% Pulp (based on mass of the entire suspension), and at a concentration of the liquor of more than 5 wt.%. , preferably 9 wt.% (based on the mass of the solution), carried out.
  • a particularly interesting embodiment of a cold alkaline extraction is that, during the treatment of the pulp with the lye, the pulp consistency is brought to more than 10% by weight, preferably more than 30% by weight pulp, a lye content of less than 7% by weight. is adjusted to solution and the solution to temperatures of less than -10 ° C, preferably -15 ° C to -20 ° C is cooled. This method is referred to below as "freeze purification".
  • This method is based on the phenomenon that water freezes from the alkali during freezing, whereby the remaining liquor is concentrated higher. As a result, the lye concentration can be significantly reduced, without the cleaning effect is impaired.
  • a further preferred embodiment of the method according to the invention is characterized in that the extraction step is a hot alkali extraction, wherein the treatment of the pulp with caustic, at a temperature of more than 80 ° C, preferably 110 ° C is performed.
  • the treatment of the pulp with lye is preferred at a pulp density of more than 5% by weight, preferably 10% by weight of pulp (based on the mass of the entire suspension), and at a lye concentration of more than 3% by weight. , preferably more than 5 wt.% (Based on solution) performed.
  • a particularly preferred embodiment of the method according to the invention is characterized in that the pulp is subjected to both a cold-alkali extraction and a hot-alkali extraction. This is particularly favorable, especially in the processing of pulps from an acidic bisulfite pulping.
  • the content of gamma-cellulose is advantageously less than 40 g / l, preferably less than 20 g / l of liquor.
  • the process according to the invention can be carried out advantageously in particular when an acid bisulfite process is used as the digestion process.
  • the present invention also relates to the use of a chemical pulp produced according to the method of the invention as starting material for the production of lyocell moldings, cellulose acetate moldings and cellulose ethers.
  • lyocell moldings are meant cellulosic molded articles which are produced by the so-called amine-oxide process, i. by dissolving pulp in an aqueous solution of a tertiary amine oxide, shaping the solution and precipitating out of the shaped solution.
  • the pulp produced according to the invention when used for the production of lyocell molded bodies, it should preferably have a viscosity of 350-550 ml / g, preferably 350-450 ml / g, a pentosan content of less than 2% by weight, preferably less than 1% by weight. %, and have an R18 content of more than 94% by weight, preferably more than 95% by weight.
  • R18 content is understood by the person skilled in the art as the filterable residue after treatment with 18% strength lye (according to DIN 54355).
  • pulps which have been obtained by means of an acidic bisulphite digestion and have been purified by means of at least one cold and one hot alkali extraction each yield outstanding values with regard to the strength properties of lyocell fibers produced therefrom.
  • Such lyocell moldings produced in this way are also distinguished by a significantly lower proportion of hemicelluloses.
  • the content of pentosan in the lyocell moldings according to the invention is preferably 1.5% by weight and less, more preferably 1% by weight and less.
  • the strength properties of lyocell fibers made in this way are in the same range as those of fibers from a prehydrolysis kraft pulp. This was not possible using a pulp derived from an acidic bisulfite process.
  • the pulp produced according to the invention should preferably have a viscosity of more than 450 ml / g, preferably 500-600 ml / g, a pentosan content of less than 2% by weight, preferably less than 1% by weight. %, and have an R18 content of more than 95% by weight, preferably more than 96% by weight.
  • the pulp produced according to the invention when used for the production of cellulose ethers, in particular for the preparation of methylcellulose, hydroxypropylmethylcellulose and hydroxyethylcellulose, it should preferably have a viscosity of 230-300 ml / g, preferably 250 ml / g, a pentosan content of less than 2% by weight. %, preferably less than 1% by weight, and have an R18 content of more than 94% by weight, preferably more than 95% by weight.
  • pulps were purified from an acidic bisulfite digest which was purified by both cold caustic extraction and hot caustic extraction without a washing step between the two extraction steps (in which case the residual alkali from the cold caustic extraction serves as the alkali source in the hot alkali extraction), are excellent for the production of high purity, low molecular weight cellulose ethers.
  • an unbleached, washed pulp 1 obtained from hardwood by means of an acid bisulfite pulping is pressed in a press 2 to a consistency of more than 30% by weight, preferably 35% by weight.
  • the viscosity of the pulp is, for example, from 220-550 ml / g when it is to be used for the production of lyocell moldings or for the production of low molecular weight, high purity cellulose ethers or 500-800 ml / g when used for the production of cellulose acetate should.
  • the squeezed liquid 3 containing organic and inorganic substances from the spent sulfite liquor is returned to the recovery loop.
  • CCE tank 5 cold alkali cleaning tank 5
  • the aqueous alkaline pulp suspension is thoroughly mixed in CCE tank 5 at residence times of 10 to 120 minutes, preferably 50 minutes, and at temperatures of 10 to 50 ° C., preferably 25 ° C.
  • the thus treated pulp suspension 6 is fed to the second press 7, in which the alkali-soluble short-chain carbohydrates are separated from the solid phase.
  • the pulp consistency should be between 30 to 40% by weight, preferably 35% by weight.
  • the press cake 8 is scraped off, diluted to a lower consistency and fed to further process steps.
  • Such further process steps include, for example, a hot alkali extraction (with or without a washing step between the two alkali extraction steps), oxygen delignification and / or chlorine dioxide treatment and optionally bleaching treatments.
  • a portion of the pressing liquor 9 is passed through a filter 10 to remove fibers and undissolved particles, and then treated in a membrane separation process by means of, for example, an ultrafiltration or nanofiltration apparatus 11.
  • part of the pressing liquor 23 can be recycled directly to the CCE tank 5.
  • the pressure-driven membrane separation system removes the dissolved polymeric and oligomeric carbohydrate degradation products.
  • the efficiency of the removal depends on the cut-off of the membrane system used. In the case of nanofiltration with cut-offs of ⁇ 1000 g / mol, significant fractions of gamma-cellulose are retained.
  • This closed loop allows the recovery of a significant portion of the alkali needed for cold caustic extraction.
  • the ratio between retentate and permeate is preferably kept between 2 and 5, in particular between 4 and 5. In the latter case, a NaOH recovery in the permeate of 80-83% can be achieved.
  • the retentate 13 containing more than 100 g / l of hemicellulose is pumped to a mixing tank 16 in which reagents 17, e.g., surfactants and / or polyelectrolytes, are added to precipitate the high molecular weight fraction (beta-cellulose).
  • reagents 17, e.g., surfactants and / or polyelectrolytes are added to precipitate the high molecular weight fraction (beta-cellulose).
  • the phase separation may be completed in a sedimentation tank 18 or by other suitable means (not shown here, e.g., microfiltration, etc.).
  • the precipitate 19, which is characterized as a high molecular weight hemicellulose fraction (beta-cellulose), can be further purified to give different degrees of purity.
  • the beta-cellulose-free supernatant 20 may either be returned to the caustic for alkali extraction or used as a source of gamma-cellulose 21.
  • the proportion of beta-cellulose can be reduced by a thermal treatment 22 of the pressing liquor.
  • a thermal treatment 22 of the pressing liquor When thermally treated for 30 minutes at 90 ° C, a 50% conversion of beta-cellulose to gamma-cellulose was observed.
  • Pulp was subjected to cold caustic extraction using fresh liquor, a liquor containing 20 g / l gamma-cellulose, and a liquor containing 14 g / l beta-cellulose and 24 g / l gamma-cellulose, each at different concentrations were used.
  • the pentosan content of the treated pulp was determined.
  • FIG. 2 shows the influence of the respective proportions of dissolved beta and gamma-cellulose on the residual content of pentosan in the pulp.
  • UABD pulp unbleached beech pulp obtained by means of an acidic bisulfite pulping was prepared according to the method described in US Pat FIG. 1 dehydrated to a consistency of 35 wt.% And subjected to a cold-alkali extraction (100 g / l NaOH, 25 ° C, residence time 30 min).
  • the chemical properties of the starting pulp are described in the following table: cellulose unit value Kappa 5.7 intrinsic viscosity ml / g 519 Alpha-cellulose % 92.6 Beta-cellulose % 6.1 Gamma-cellulose % 1.3 After leaving the CCE reactor, the alkaline pulp suspension was squeezed to a consistency of 32% by weight.
  • the necessary addition of fresh liquor may even increase by 409 kg NaOH / tonne pulp in the case of a target concentration of ⁇ 1 g / l beta-cellulose (Example 3c compared to Example 3a) or by 276 kg NaOH / t otro pulp in the case of a target concentration of ⁇ 5 g / l beta-cellulose (Example 3f compared to Example 3d) can be reduced.
  • the carry over liquor to the HCE stage was measured and, assuming that the pulp was dewatered to a consistency of 32%, was calculated to be 240 kg / t dry pulp.
  • Such low viscosity cellulose ethers are suitable for use as coatings and protective colloids in emulsion polymerization reactions which require pulps or cotton linters having an intrinsic viscosity of about 250 ml / g.
  • a UBABD pulp was subjected to the following treatment and bleaching sequences: CCE-W-HCE / OZP and HCE / OW-CCE-ZP, respectively.
  • Mean "CCE” a cold alkaline extraction "W” an intermediate wash
  • HCE a hot alkaline extraction
  • O an oxygen delignification
  • Z an ozone bleaching stage
  • P is a peroxide bleach stage.
  • the (E / O) -Z-P sequence was performed under both standard conditions (i.e., mild conditions) and under enhanced conditions.
  • pulps viscosity HCE CCE stage Z stage P-stage OXE category bleaching sequence NaOH c-NaOH Beta Gamma H 2 SO 4 O 3 NaOH H 2 O 2 ml / g Bleaching yield (%) kg / tZ g / l g / l g / l kg / tZ kg / tZ kg / t kg / t kg / t Beech sulfite EO-ZP (standard) 610 91.7 24 6 4.2 4.0 0.7 564 Beech sulfite EO-ZP (HCE-enhanced) 610 82.0 96 6 3.6 4.0 1.2 521 Eucalyptus PHK *) OO-AZP (standard) 756 97.0 15 2.6 7.2 11.0 972 Beech sulfite CCE-W-HCE / OZP 519 89.1 30 100 0 0 6
  • the pulp was also processed according to the sequence CCE-W-HCE / OZP, but the liquor used for CCE treatment was (a) with 20 g / l gamma-cellulose or (b) with 20 g / l beta Cellulose contaminated.
  • the pulps were processed in a conventional manner to Lyocell fibers with a titer of 1.3 dtex.
  • lyocell fibers made from both CCE and HCE treated UBABD pulp have strengths comparable to those of eucalyptus PHK pulp. These strengths are significantly higher than those achieved with UBABD pulp fibers made without CCE treatment.
  • the combination of a CCE and an HCE treatment thus results in UBABD pulps which can be used excellently for the production of lyocell fibers, which fibers have strengths that heretofore were achievable only by the use of prehydrolysis kraft pulps.
  • Fibers from a pulp treated in the above case (a) with a gamma-cellulose contaminated CCE liquor showed no significant variation in strength.
  • a lyocell fiber made of a pulp treated with a beta-cellulose-contaminated CCE liquor (Case (b) above) has lower strength.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
EP05741840.2A 2004-06-02 2005-05-20 Verfahren zur herstellung eines chemiezellstoffes Active EP1753908B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT9532004A AT413548B (de) 2004-06-02 2004-06-02 Verfahren zur herstellung eines chemiezellstoffes und seine verwendung
PCT/AT2005/000171 WO2005118950A1 (de) 2004-06-02 2005-05-20 Verfahren zur herstellung eines chemiezellstoffes

Publications (2)

Publication Number Publication Date
EP1753908A1 EP1753908A1 (de) 2007-02-21
EP1753908B1 true EP1753908B1 (de) 2016-02-03

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EP (1) EP1753908B1 (no)
AT (1) AT413548B (no)
CA (1) CA2568594C (no)
NO (1) NO338462B1 (no)
WO (1) WO2005118950A1 (no)
ZA (1) ZA200610044B (no)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT503611B1 (de) * 2006-05-10 2009-05-15 Chemiefaser Lenzing Ag Verfahren zur herstellung eines zellstoffes
AT503610B1 (de) * 2006-05-10 2012-03-15 Chemiefaser Lenzing Ag Verfahren zur herstellung eines zellstoffes
AT503612A1 (de) * 2006-05-10 2007-11-15 Chemiefaser Lenzing Ag Verfahren zur herstellung eines zellstoffes
JP2015518248A (ja) 2012-04-26 2015-06-25 レンツィング アクチェンゲゼルシャフト 電池セパレータ
FI129086B (en) * 2012-09-14 2021-06-30 Teknologian Tutkimuskeskus Vtt Oy Method for producing soluble pulp
ES2667994T3 (es) 2013-02-22 2018-05-16 Lenzing Aktiengesellschaft Separador de batería
CN104611973A (zh) * 2013-11-04 2015-05-13 新疆光大山河化工科技有限公司 一种精制棉黑液处理工艺
EP3347522B1 (en) * 2015-09-07 2020-06-17 Domsjö Fabriker AB Novel dissolving pulp
JP2017224611A (ja) * 2017-07-06 2017-12-21 レンツィング アクチェンゲゼルシャフト 電池セパレータ
SE1850733A1 (en) * 2018-06-15 2019-12-16 Valmet Oy Method and assembly for optimizing filtrate circulation in a kraft process
SE2250793A1 (en) * 2022-06-27 2023-12-28 Valmet Oy Method for processing cellulose pulp obtained from a kraft process

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI49438C (fi) * 1973-07-23 1980-12-23 Keskuslaboratorio Foerfarande foer avlaegsnande av hemicellulosa ur hemicellulosahaltiga alkaliloesningar i processcirkulation
US4270914A (en) * 1979-10-26 1981-06-02 Borregaard Industries Limited Process for controlling hemicellulose concentration during the mercerization of cellulose
US5589053A (en) * 1995-11-03 1996-12-31 Huron Tech Incorporated Electrolysis process for removal of caustic in hemicellulose caustic
WO1997023279A1 (de) * 1995-12-23 1997-07-03 Krebs & Co. Ag Verfahren zur reinigung einer mit fadenmolekülen verschmutzten flüssigkeit

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WO2005118950A1 (de) 2005-12-15
NO338462B1 (no) 2016-08-22
ATA9532004A (de) 2005-08-15
EP1753908A1 (de) 2007-02-21
ZA200610044B (en) 2008-02-27
NO20065354L (no) 2007-01-31
AT413548B (de) 2006-03-15
CA2568594C (en) 2013-07-16
CA2568594A1 (en) 2005-12-15

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