EP0498330A1 - Verfahren zum Delignifizieren von Pflanzenfasermaterial - Google Patents

Verfahren zum Delignifizieren von Pflanzenfasermaterial Download PDF

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Publication number
EP0498330A1
EP0498330A1 EP92101701A EP92101701A EP0498330A1 EP 0498330 A1 EP0498330 A1 EP 0498330A1 EP 92101701 A EP92101701 A EP 92101701A EP 92101701 A EP92101701 A EP 92101701A EP 0498330 A1 EP0498330 A1 EP 0498330A1
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EP
European Patent Office
Prior art keywords
delignification
impregnation
alcohol
stage
fiber material
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.)
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Application number
EP92101701A
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German (de)
English (en)
French (fr)
Inventor
Karl-Heinz Brodersen
Gerhard Dahlmann
Heinrich Dr. Leopold
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.)
Organocell Gesellschaft fur Zellstoff- und Umwelttechnik Mbh
Original Assignee
Organocell Gesellschaft fur Zellstoff- und Umwelttechnik Mbh
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Publication date
Application filed by Organocell Gesellschaft fur Zellstoff- und Umwelttechnik Mbh filed Critical Organocell Gesellschaft fur Zellstoff- und Umwelttechnik Mbh
Publication of EP0498330A1 publication Critical patent/EP0498330A1/de
Withdrawn legal-status Critical Current

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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
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • 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 delignifying plant fiber material, in particular wood chips, using alcohol.
  • ORGANOSOLV processes are processes in which alcohol is preferably used as the delignifying agent. These processes avoid the use of sulfur compounds, the main disintegrant used today.
  • the SULFAT process which is in first place today, requires the use of sulfide for delignification, which leads to environmentally harmful air emissions. In addition, the process has significant odor nuisance.
  • the SULFIT process is somewhat easier to control than the SULFAT process, but the pulp produced in the SULFIT process is below the sulfate pulp in terms of its strength values.
  • Particularly good pulp qualities could be achieved by using a two-stage process in which the chips were boiled in an acidic alcohol-water mixture in the first stage, followed by a second stage in which the alcohol-water was added Mixture of sodium hydroxide solution and alcohol was added and the cooking continued in the alkaline range.
  • the boiling process was preceded by an impregnation in which the wood chips were first heated by steam and then impregnated in an alcohol-water mixture at a lower temperature.
  • pure alcohol or an alcohol / water mixture is added to the plant fiber material in the impregnation stage, which / which has an elevated temperature or is brought to an elevated temperature.
  • pure alcohol or an alcohol-water mixture is used depends on the dry content of the plant fiber material used and the desired liquor ratio. In the case of continuous processes, the lowest possible liquor ratio is generally sought.
  • the plant fiber material is left in the impregnation stage until a phase equilibrium has occurred between the added impregnation liquid and the liquid contained in the plant fiber material. This is followed by delignification by treating the impregnated plant fiber material with an alkali-alcohol-water mixture which is at an elevated temperature or which is brought to an elevated temperature so that the delignification reaction begins.
  • the amount of the alkali-alcohol-water mixture depends on the cooking process, whether continuous or discontinuous, in particular on the amount of impregnating liquid introduced into the delignification step.
  • an alkali / water mixture is constantly added to the delignification stage.
  • the delignification itself is carried out in such a way that the alcohol contained in the plant fiber material decreases approximately uniformly during the delignification and the alkali fraction in the plant fiber material increases at the beginning of the delignification and decreases during the delignification until approximately a phase equilibrium has occurred again.
  • the impregnation step and the delignification step can be carried out successively in a cooker container, i.e. the plant fiber material is introduced into the container and the impregnation with the alcohol-water mixture is carried out first; the alkali-water mixture can then be introduced into the container and the delignification can be carried out.
  • the preferred embodiment provides for the impregnation liquid to be removed from the container and then for the delignification liquid to be introduced and for the delignification to be carried out.
  • This variant opens up the possibility of a lower use of alkali.
  • the impregnation stage and the delignification stage are locally arranged one after the other in one or two containers. While only the liquids are moved in the discontinuous process, the plant fiber material is also moved in the continuous process.
  • the amount of alcohol added to the plant fiber material in the impregnation stage is selected so that the alcohol component in the impregnation liquid is 30-60% by weight, in particular 40-50% by weight.
  • the plant fiber material With the plant fiber material, a not insignificant amount of liquid, depending on the dry content of the plant fiber material, is introduced into the impregnation stage.
  • An appropriate amount of alcohol and alcohol concentration must be selected so that the phase balance required in the impregnation stage is established; this means that at the beginning of the impregnation the alcohol content in the impregnation liquid is briefly above the desired proportion.
  • the highest possible proportion of alcohol in the impregnation liquid is advantageous with regard to the rapid penetration of the alcohol into the wood chips.
  • the delignification following the impregnation is to be carried out with a smaller amount of alcohol in the delignification liquid than in the impregnation liquid, so that the delignification carried out in the delignification stage is not impeded by the excessive alcohol content. It is advantageous if the alcohol content is 20-40% by weight, in particular 20-30% by weight, based on the delignification liquid.
  • the alkali fraction should make up 12-25% by weight, in particular 18-20% by weight for long fiber material and 14-18% by weight for short fiber material, based on dry plant fiber material. The alkali portion used results in a favorable delignification of the plant fiber material.
  • Methanol or ethanol is preferably used as the alcohol. These alcohols are preferable to other alcohols because of their boiling temperature and low heat content.
  • a sodium hydroxide solution is used as the alkali.
  • the temperature of the impregnation liquid is 100-160 ° C, in particular 110-130 ° C, it is chosen so that the impregnation does not take too long a period without a visible delignification already occurring.
  • the temperature of the delignification liquid is selected depending on the type of plant fiber material. It is 150-190 ° C, especially 160-175 ° C. Easier digestible plant fiber materials are treated at lower temperatures, while harder digestible plant fiber materials are delignified at higher temperatures.
  • the residence time in the impregnation is 30-120 min. preferably 60 min.
  • a longer period of time is provided for the delignification, which is between 100-300 minutes, preferably 150 minutes.
  • the impregnating liquid and the delignifying liquid are heated indirectly in a separate heating circuit; that is, the same heating circuit can be used for both impregnation and delignification.
  • a separate heating circuit can be provided for heating the impregnating liquid and the delignifying liquid. It is advantageous if the impregnation liquid with the vegetable fiber material is introduced into the impregnation stage in the continuous process. For this purpose, part of the impregnation liquid is continuously drawn off at the lower end of the impregnation stage, heated by a heat exchanger and the plant fiber material flow added before the impregnation begins.
  • the liquor ratio i.e. the ratio of liquid to the plant fiber material used, special importance. In the impregnation stage, this liquor ratio is chosen so that it is 2: 1 to 3.5: 1, preferably 2.2: 1.
  • the liquor ratio is 3.5: 1 to 5: 1, preferably 4.5: 1.
  • the pH of the impregnation stage is 4-6 and in the boiling stage 9-12.
  • an additional improvement of the process can be achieved by adding a small amount of alkali to the impregnation step.
  • a particularly favorable mode of operation is obtained if the digestion liquid and the plant fiber material are passed through the delignification stage in cocurrent in the continuous process.
  • the delignification liquid is drawn off and fed to an alcohol recovery system in which the alcohol is concentrated to 95%.
  • the delignifying liquid is heated via the amount of alkali water which is added to the vegetable fiber and impregnating liquid mixture coming from the impregnation stage.
  • the plant fiber material is subjected to a countercurrent wash in order to remove the amounts of alcohol and alkali still present in the plant fiber material, which is already pulp.
  • anthraquinone is added in an amount of 0.01-0.15% by weight to atro plant fiber material during the delignification, in order thereby to further improve the degree of disintegration during the delignification.
  • the impregnation stage is preceded by a damping of the plant fiber material.
  • the damping removes the air contained in the plant fiber material and supports the impregnation with alcohol. Steam and / or alcohol vapor can be used for damping.
  • the plant fiber material is introduced via a feed line 2 with the liquid (water) normally present in it by a corresponding entry, which is not shown in the block diagram.
  • the impregnation liquid through the line 3.
  • the plant fiber material has previously been steamed in steaming stage 4 and has a temperature of approx. 100 ° C when entering impregnation stage 1.
  • the steaming removed the air from the wood chips.
  • the alcohol introduced into the impregnation stage 1 comes through line 5 from an alcohol recovery system, which has been omitted for the sake of clarity, and is 95% pure. The remaining 5% is water.
  • impregnation stage 1 the impregnation liquid and thus also the plant fiber material are heated in a very short time from 100 ° C. to 140 ° C. (FIG. 2).
  • the heat exchanger 6 is provided for heating the impregnation liquid.
  • part of the impregnation liquid is drawn off, fed to the heat exchanger 6 and fed back to the impregnation stage 1 at the entry end 8.
  • the impregnation temperature and the alcohol concentration of the impregnation liquid are kept as constant as possible during the entire impregnation process.
  • the alcohol concentration in the impregnation liquid will be approximately constant over the largest range of the impregnation time. A higher concentration is only present at the beginning of the impregnation, as can be seen in FIG. 3.
  • the alcohol concentration increases continuously until the phase equilibrium between the alcohol concentrations occurs towards the end of the impregnation.
  • the plant fiber material with the liquid of alcohol and water contained therein and a predeterminable amount of impregnation liquid is fed via line 9 to the delignification stage 10.
  • the alkali-water mixture is also introduced through line 11;
  • the temperature of the plant fiber material and the delignification liquid in the delignification stage 10 increases from 140 ° C to 165 ° C.
  • the delignification liquid is heated via the heat exchanger 12.
  • the addition of the alkali with the simultaneous heating has the result that the amount of alcohol in the delignification stage 10 is also reduced at the same time and the delignification begins.
  • the alcohol concentration in the liquid is reduced from 50% to 33% in a very short time in order to remain roughly constant afterwards.
  • the alcohol concentration in the wood chips decreases approximately evenly over the entire time of the deliginification stage until phase equilibrium is restored at 33% (FIG. 4).
  • the alkali introduced into the liquid reduces its concentration from 5% to approx. 3%, by mixing with the liquid present from the impregnation stage very quickly, and then to decrease continuously to approx. 1.5%.
  • the alkali penetrates into the fibrous material in a uniformly constant manner, as shown in FIG.
  • the phase balance is set at around 1.5%.
  • the delignification stage is then ended.
  • the alkali consumed during the delignification is compensated for by appropriate addition of alkali through the line 13 coming from the chemical recovery.
  • a wash 14 is connected to the delignification in order to remove the remaining alcohol and alkali parts from the pulp resulting from the delignification.
  • the diagrams show the main course of the temperatures and the amounts of chemicals. It goes without saying that, depending on the plant fiber material, alkali and alcohol used, deviations in the course of the curves can occur here, but the basic structure of the curves is retained.
  • the alkali and alcohol are washed out of the pulp and fed with the washing liquid via line 15 to a chemical recovery.
  • the delignification liquid is also drawn off via line 15 and fed into the alcohol recovery with subsequent evaporation.

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  • Paper (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Fertilizers (AREA)
EP92101701A 1991-02-06 1992-02-03 Verfahren zum Delignifizieren von Pflanzenfasermaterial Withdrawn EP0498330A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4103572A DE4103572C2 (de) 1991-02-06 1991-02-06 Verfahren zum Delignifizieren von Pflanzenfasermaterial
DE4103572 1991-02-06

Publications (1)

Publication Number Publication Date
EP0498330A1 true EP0498330A1 (de) 1992-08-12

Family

ID=6424485

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92101701A Withdrawn EP0498330A1 (de) 1991-02-06 1992-02-03 Verfahren zum Delignifizieren von Pflanzenfasermaterial

Country Status (16)

Country Link
US (1) US5470433A (un)
EP (1) EP0498330A1 (un)
JP (1) JPH0551886A (un)
KR (1) KR920016651A (un)
AR (1) AR246568A1 (un)
AU (1) AU654997B2 (un)
BR (1) BR9200401A (un)
CA (1) CA2060798A1 (un)
CS (1) CS30292A3 (un)
DE (1) DE4103572C2 (un)
FI (1) FI920493A (un)
NO (1) NO178406C (un)
NZ (1) NZ241401A (un)
PL (1) PL293377A1 (un)
PT (1) PT100096A (un)
ZA (1) ZA92466B (un)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0777780B1 (de) * 1994-08-26 1998-11-18 IMPCO-VOEST-ALPINE PULPING TECHNOLOGIES GmbH Sulfitaufschlussverfahren
WO2012054947A3 (de) * 2010-10-29 2012-08-23 Annikki Gmbh Verfahren zur gewinnung von lignin

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4343508C2 (de) * 1993-12-20 1997-08-07 Eugen Edel Chemo-thermo-mechanisches Verfahren zur Herstellung von Zellstoff aus Pflanzenfasermaterial
US5650045A (en) * 1994-12-14 1997-07-22 Salminen; Reijo K. Apparatus and method for wood pulp digester
DE19704054C2 (de) 1997-02-04 2000-08-10 Stockhausen Chem Fab Gmbh Verfahren zur Herstellung von Faserstoffen mit verbesserten Eigenschaften
US6306248B1 (en) 1997-11-20 2001-10-23 The University Of Alabama In Huntsville Method for transforming diverse pulp and paper products into a homogenous cellulosic feedstock
US6923887B2 (en) * 2003-02-21 2005-08-02 Alberta Research Council Inc. Method for hydrogen peroxide bleaching of pulp using an organic solvent in the bleaching medium
FI122838B (fi) * 2005-03-31 2012-07-31 Metso Paper Inc Menetelmä massan valmistamiseksi lignoselluloosamateriaalista
AU2007275036A1 (en) 2006-07-21 2008-01-24 Xyleco, Inc. Conversion systems for biomass
JP2010527619A (ja) * 2007-05-31 2010-08-19 リグノル イノヴェイションズ リミテッド リグノセルロース系原料の連続向流オルガノソルブ処理
WO2009021216A2 (en) * 2007-08-08 2009-02-12 Bountiful Applied Research Corp. Lignin dewatering process
TWI676687B (zh) * 2009-08-06 2019-11-11 奧地利商安尼基有限公司 用以由木質纖維素材料製造醣類裂解產物之方法
JP2013042727A (ja) * 2011-08-26 2013-03-04 Kawasaki Heavy Ind Ltd リグノセルロース系バイオマスからエタノールを製造する方法及びその前処理方法
KR101395053B1 (ko) * 2012-02-28 2014-05-20 경상대학교산학협력단 식물성 바이오매스로부터 글루코오스의 생산 방법
WO2015075080A1 (en) 2013-11-20 2015-05-28 Annikki Gmbh Process for fractionating lignocellulosics
DE102015108222A1 (de) 2015-05-26 2016-12-01 Hochschule Magdeburg-Stendal Verfahren zur Abtrennung von Lignin aus Biomassen und daraus gewonnene Stoffe
SE539761C2 (en) 2016-03-21 2017-11-21 Stora Enso Oyj Liquid lignin composition, lignin-based resin, and method of increasing the solubility of equation

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0012960A1 (de) * 1978-12-20 1980-07-09 MD Papier GmbH & Co. KG Verfahren und Vorrichtung zum kontinuierlichen Aufschliessen von Pflanzenfasermaterial
EP0090969A1 (de) * 1982-04-06 1983-10-12 MD-Organocell Gesellschaft für Zellstoff- und Umwelttechnik mbH Verfahren und Reaktor zum kontinuierlichen Aufschliessen von Pflanzenfasermaterial

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3585104A (en) * 1968-07-29 1971-06-15 Theodor N Kleinert Organosolv pulping and recovery process
CA1079008A (en) * 1975-10-24 1980-06-10 Cp Associates Limited Solvent pulping process
AT385061B (de) * 1985-11-29 1988-02-10 Neusiedler Ag Verfahren zur gewinnung von zellstoff aus pflanzenfasermaterial

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0012960A1 (de) * 1978-12-20 1980-07-09 MD Papier GmbH & Co. KG Verfahren und Vorrichtung zum kontinuierlichen Aufschliessen von Pflanzenfasermaterial
EP0090969A1 (de) * 1982-04-06 1983-10-12 MD-Organocell Gesellschaft für Zellstoff- und Umwelttechnik mbH Verfahren und Reaktor zum kontinuierlichen Aufschliessen von Pflanzenfasermaterial

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
TAPPI JOURNAL. Bd. 73, Nr. 4, April 1990, ATLANTA US Seiten 237 - 240; DAHLMANN, G. ET AL.: 'The Organocell process-pulping with the environment in mind.' *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0777780B1 (de) * 1994-08-26 1998-11-18 IMPCO-VOEST-ALPINE PULPING TECHNOLOGIES GmbH Sulfitaufschlussverfahren
WO2012054947A3 (de) * 2010-10-29 2012-08-23 Annikki Gmbh Verfahren zur gewinnung von lignin

Also Published As

Publication number Publication date
AU654997B2 (en) 1994-12-01
NZ241401A (en) 1994-09-27
NO920459L (no) 1992-08-07
BR9200401A (pt) 1992-10-13
US5470433A (en) 1995-11-28
PT100096A (pt) 1993-04-30
KR920016651A (ko) 1992-09-25
FI920493A (fi) 1992-08-07
CA2060798A1 (en) 1992-08-07
AU1075592A (en) 1992-08-13
NO920459D0 (no) 1992-02-04
JPH0551886A (ja) 1993-03-02
PL293377A1 (en) 1992-10-19
DE4103572A1 (de) 1992-08-13
NO178406C (no) 1996-03-20
CS30292A3 (en) 1992-08-12
DE4103572C2 (de) 1995-11-23
FI920493A0 (fi) 1992-02-05
NO178406B (no) 1995-12-11
ZA92466B (en) 1993-10-07
AR246568A1 (es) 1994-08-31

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