EP0777780B1 - Sulfitaufschlussverfahren - Google Patents

Sulfitaufschlussverfahren Download PDF

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Publication number
EP0777780B1
EP0777780B1 EP95928394A EP95928394A EP0777780B1 EP 0777780 B1 EP0777780 B1 EP 0777780B1 EP 95928394 A EP95928394 A EP 95928394A EP 95928394 A EP95928394 A EP 95928394A EP 0777780 B1 EP0777780 B1 EP 0777780B1
Authority
EP
European Patent Office
Prior art keywords
digestion
process according
solution
raw material
impregnating
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 - Lifetime
Application number
EP95928394A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0777780A1 (de
Inventor
Karl Fuchs
Albert Huber
Hans-Ludwig Schubert
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.)
Impco-Voest-Alpine Pulping Technologies GmbH
Original Assignee
Impco-Voest-Alpine Pulping Technologies GmbH
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 Impco-Voest-Alpine Pulping Technologies GmbH filed Critical Impco-Voest-Alpine Pulping Technologies GmbH
Publication of EP0777780A1 publication Critical patent/EP0777780A1/de
Application granted granted Critical
Publication of EP0777780B1 publication Critical patent/EP0777780B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/06—Pretreatment of the finely-divided materials before digesting with alkaline reacting 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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing 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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
    • 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
    • D21C3/22—Other features of pulping processes
    • D21C3/222—Use of compounds accelerating the pulping processes

Definitions

  • the present invention relates to a sulfite digestion process for the production of pulps using alkaline Monosulfite solutions, organic solvents and quinone derivatives.
  • the raw materials are essentially in the sulfite digestion process (shredded wood) in an acidic or neutral setting Cooking acid introduced and this contain lignocellulose Materials cooked with solutions of hydrogen sulfites or sulfites. If the hydrogen sulfite solutions additionally sulfur dioxide contain, one speaks of "acid bisulfite process".
  • An alkaline sulfite digestion solution generally consists of a sulfite and carbonates or bases; the specific digestion variant is always dependent on the one used Type of wood.
  • EP-A1-0 538 576 and AT-B-398 992 each disclose methods for recovering the chemicals used for pulping from the waste liquor according to the ASAM method.
  • the waste liquor is burned in an alkali combustion boiler, the slag or ash is drawn off, dissolved in water, converted to H 2 S and burned, sodium sulfite being recovered from the waste gases formed during the combustion.
  • EP-0 498 330 A1 describes an impregnation step for use disclosed in a strictly sulfur-free digestion process. According to column 1, lines 10 to 12 it is stated that ORGANOSOLV procedure - and the procedure of this document is one such - avoid the use of sulfur compounds.
  • the object of the present invention is one the described prior art further improved sulfite digestion process to provide which one is more efficient Digestion of the raw material, improved recovery of substances used as well as a process engineering Simplifies the procedure.
  • this object is achieved by a sulfite process lignocellulosic raw material using water soluble alkaline monosulfite solutions, organic solvents and at least one quinone derivative, in which the raw material before the actual digestion of the raw material an impregnation step without organic solvents in the presence of the monosulfite solution and optionally the Quinone derivative at a temperature below that for the digestion reaction is the required temperature becomes.
  • the quinone derivative can be used during the impregnation of the pipe material be present, or will with the other components still missing for digestion.
  • the Quinone derivative accelerates in alkaline digestion processes Redox catalyst delignifies and stabilizes the reducing ones Ends the carbohydrates against an alkaline "peeling off".
  • a preferred quinone derivative is anthraquinone.
  • the organic solvent is only after this impregnation step added to the alkaline monosulfite solution.
  • Said raw material is used for a period of 5 to 360 min, preferably from 15 to 60 min, with the alkaline monosulfite solution impregnated.
  • the ones usually used Temperatures are between 60 and 150 ° C, preferably between 100 and 130 ° C.
  • the impregnation with the alkaline monosulfite solution can be ended be by the organic solvent or the solvent / water mixture entered in the impregnating solution becomes.
  • the ionic strength of the impregnating liquor should by the entry of the organic solvent or Solvent / water mixture to the necessary for the digestion Concentration can be adjusted.
  • the solvent e.g. low-boiling alcohols, such as methanol
  • the solvent can after the impregnation of the digestion material under pressure in the digestion system can be entered. Then that will Digestion material with the complete digestion solution to the Reaction required temperature heated, or the impregnation is carried out using modern displacement technology a complete digestion solution containing the solvent exchanged.
  • Impregnation solution that has a higher ion concentration than the actual one Has digestion solution. This requires a faster one and more homogeneous distribution of the alkaline and monosulfitic Digestion chemicals in the digestion material.
  • the impregnation liquor can either be compared to that used for cooking required quantities with an excess of inorganic Chemical and liquid quantities are used, or with the chemical quantities required for the digestion in comparison for cooking reduced liquid volume.
  • the solvent or solvent-water mixture can act as a displacement medium be used.
  • the repressed or deducted Displacement can be done with fresh chemicals on the Initial concentration can be strengthened and reused.
  • the solvent used for the displacement can be mixed with water be offset so that the chemicals required for digestion and solvent concentration can be set variably. An energy saving due to the lower requirements the purity and concentration of the recovered solvent, becomes possible.
  • the impregnation can be carried out with less liquid be considered necessary for the digestion itself. It However, it must be ensured that all digestion material is soaked. This can e.g. by pumping around the impregnation solution can be achieved. In the impregnation the digestion material takes the inorganic digestion chemicals. The chemical concentration the digestion solution is at the end of the impregnation by replenishing the solvent or the solvent-water mixture to those necessary for the digestion Concentration adjusted or by displacing the impregnation solution achieved with complete digestion solution.
  • This process design has the technological advantage that the solvent-based lye circuit on the areas the digestion system, the black liquor management up to the solvent separation as well as parts of the brown cloth wash limited remains.
  • the white liquor remains solvent-free, which increases its solubility the inorganic digestion chemicals is increased.
  • the impregnation step can be replaced (e.g. by displacing) the impregnation solution with the digestion solution will.
  • an aqueous solution of the inorganic Digestion chemicals possibly together with the one to be used Quinone derivative, filled in the stove, the stove heated to maximum temperature and the digestion carried out will.
  • the heating time can be compared to normal digestion be shortened very much because of the improved Woodiness of the inorganic digestion chemicals penetrate very quickly into the microstructure of the wood.
  • the Total cook time is not extended.
  • the maximal Digestion temperature can e.g. for softwood from 180 to 173 - Reduced 170 °, which causes the stove pressure to be dependent reduced by the solvent content of the digestion solution.
  • the solvent should preferably be used during the digestion reaction in an amount between 0.5 and 50 percent by volume of the total Amount of liquid should be present.
  • Sodium sulfite is preferred in the alkaline monosulfite solutions in an amount between 5 and 40% based on the raw material.
  • Other bases e.g. Potassium hydroxide or potassium carbonate, but are also suitable.
  • aqueous solutions from sodium hydroxide and / or sodium carbonate to the monosulfite solutions be mixed, in an amount between 0 and 15% based on the raw material used.
  • the digestion solution and the digestion material can be directly after the or with the entry of all digestion chemicals still required to the temperature necessary for the digestion reaction to be brought.
  • the digestion process can be done by displacing the digestion solution or be finally ended by cooling the system.
  • the processes described can be both continuous and can also be operated discontinuously. Is a discontinuous If the procedure is desired, there is a preferred one Process variant in that the impregnation step already is carried out in standing, discontinuous stoves, at where the liquids are moved by pumps and the Raw materials are entered using filling equipment.
  • the impregnation solution is preferred in this case from a separate impregnation solution tank introduced into the cooker.
  • the impregnation step preferably carried out in a separate impregnation tower, and then the digestion material with a liquid transported into the cooker.
  • FIG.1 An example of a system for a continuous process is shown in Fig.1:
  • Raw material (1) is heated in a container (2) by means of steam (3, 4) and transferred into the feed system (5), in which the impregnation solution (6), which consists of NaOH, Na 2 CO 3 , Na 2 SO 3 and anthraquinone.
  • the mixture is passed via a heat exchanger (7) into the impregnation tower (8), in which the actual impregnation step takes place.
  • the impregnated raw material is fed from the impregnation tower via further heat exchangers (9, 10) into the cooking tower (12), with the solvent methanol (11) also being added between the heat exchangers (9) and (10). After the digestion phase, both the pulp (13) and the lye (14) are led out of the digester and processed or reprocessed.
  • the invention enables a significant simplification the procedure of the ASAM procedure and simplified its implementation in industrial practice, both at continuous as well as discontinuous digestion systems.
  • the splinter content is improved by impregnation of pulps is reduced and the yield of accepted substances is increased.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)
  • Processing Of Solid Wastes (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Data Exchanges In Wide-Area Networks (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
EP95928394A 1994-08-26 1995-08-25 Sulfitaufschlussverfahren Expired - Lifetime EP0777780B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT1651/94 1994-08-26
AT0165194A AT401068B (de) 1994-08-26 1994-08-26 Sulfitaufschlussverfahren
PCT/AT1995/000170 WO1996006974A1 (de) 1994-08-26 1995-08-25 Sulfitaufschlussverfahren

Publications (2)

Publication Number Publication Date
EP0777780A1 EP0777780A1 (de) 1997-06-11
EP0777780B1 true EP0777780B1 (de) 1998-11-18

Family

ID=3518027

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95928394A Expired - Lifetime EP0777780B1 (de) 1994-08-26 1995-08-25 Sulfitaufschlussverfahren

Country Status (12)

Country Link
EP (1) EP0777780B1 (pt)
CN (1) CN1160426A (pt)
AT (2) AT401068B (pt)
BR (1) BR9508634A (pt)
CA (1) CA2198485A1 (pt)
DE (1) DE59504281D1 (pt)
ES (1) ES2126305T3 (pt)
FI (1) FI970707A0 (pt)
ID (1) ID15812A (pt)
RU (1) RU2124083C1 (pt)
WO (1) WO1996006974A1 (pt)
ZA (1) ZA956506B (pt)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1325723C (zh) * 2005-03-09 2007-07-11 中国制浆造纸研究院 棉杆或灌木或枝桠材的制浆方法
ES2447375T3 (es) * 2008-12-17 2014-03-11 Borregaard As Conversión de biomasa lignocelulósica por medio de tratamiento previo con sulfito
CN104878638B (zh) * 2015-06-24 2017-09-15 济南圣泉集团股份有限公司 纤维素、木质素磺酸盐的制备方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0498330A1 (de) * 1991-02-06 1992-08-12 Organocell Gesellschaft für Zellstoff- und Umwelttechnik mbH Verfahren zum Delignifizieren von Pflanzenfasermaterial

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3518005A1 (de) * 1985-05-18 1986-11-20 Kraftanlagen Ag, 6900 Heidelberg Sulfitaufschlussverfahren zur herstellung von zellstoff aus lignozellulosehaltigen materialien mit rueckgewinnung der aufschlusschemikalien
AT398440B (de) * 1991-10-25 1994-12-27 Waagner Biro Ag Verfahren zur rückgewinnung der chemikalien der kochlauge

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0498330A1 (de) * 1991-02-06 1992-08-12 Organocell Gesellschaft für Zellstoff- und Umwelttechnik mbH Verfahren zum Delignifizieren von Pflanzenfasermaterial

Also Published As

Publication number Publication date
RU2124083C1 (ru) 1998-12-27
AT401068B (de) 1996-06-25
ATE173517T1 (de) 1998-12-15
FI970707A (fi) 1997-02-19
ES2126305T3 (es) 1999-03-16
WO1996006974A1 (de) 1996-03-07
BR9508634A (pt) 1997-12-30
FI970707A0 (fi) 1997-02-19
EP0777780A1 (de) 1997-06-11
ATA165194A (de) 1995-10-15
ZA956506B (en) 1996-03-18
DE59504281D1 (de) 1998-12-24
ID15812A (id) 1997-08-14
CN1160426A (zh) 1997-09-24
CA2198485A1 (en) 1996-03-07

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