EP0777780B1 - Sulfitaufschlussverfahren - Google Patents
Sulfitaufschlussverfahren Download PDFInfo
- 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
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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)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Data Exchanges In Wide-Area Networks (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
Aufschlußart | Standard (ASAM-Verf.) | methanolfreie Imprägnierung |
Imprägnierung | ||
Temp., °C | 120 | |
Aufheizzeit, min. | 53 | |
Zeit bei Tmax | 60 | |
MeOH, %/Flotte | 0 | |
Flotte | 3:1 | |
AQ, %/Holz | 0,1 | |
Aufschluß | ||
Temp., °C | 180 | 180 |
Aufheizzeit, min | 100 | 37 |
Zeit bei Tmax | 120 | 150 |
MeOH, %/Flotte | 15 | 15 |
Flotte | 4:1 | 4:1 |
Druckmax, bar | 14 | 14 |
Gesamtalkali (berechnet als NaOH), %Holz | 25 | 25 |
Na2 SO3: NaOH | 80:20 | 80:20 |
AQ, % Holz | 0,1 | 0,1 |
Kappa | 22,2 | 22,4 |
Gutstoffausbeute, % | 45,9 | 50,0 |
Splitter,% | 4,9 | 2,2 |
Viskosität, ml/g | 1327 | 1334 |
Weißgrad, %.ISO | 45,7 | 39,6 |
Chemikalien | 20 % Na2SO3 und 5 % NaOH berechnet als NaOH auf otro Holz |
0,075 % Anthrachinon auf otro Holz | |
15 v/v % Methanol | |
Flotte | 4:1 (Flüssigkeit:Holz) |
Technologie | Auflösen aller Chemikalien in der Flotte |
20 min Dämpfen des Aufschlußgutes | |
90 min Ankochen | |
180 min Fertigkochen bei 180°C | |
20 min Kochlauge verdrängen und Kocher entleeren | |
Ergebnis | Kappazahl: 24,6 |
Gutstoffausbeute: 47 % | |
Splitter 1,2 |
Chemikalien | 130 g/l Na2SO3 und 20 g/l NaOH (auf atro Holz) |
0,075 % Anthrachinon in der Vorimprägnierung | |
15 v/v % Methanol in der Kochung; wird erst nach der Imprägnierung zugesetzt | |
Flotte | 6:1 (Flüssigkeit:Holz) |
Technologie | Lösen der Anorganika in der Flotte |
20 min Dämpfen | |
30 min Imprägnieren bei 110°C | |
10 min Methanoleingabe und Laugenverdrängung | |
30 min Aufheizen | |
100 min Fertigkochen bei 180°C | |
20 min Kochlauge verdrängen und Kocher entleeren | |
Ergebnis | Kappazahl: 16,2 |
Gutstoffausbeute: 46,6 % | |
Splitter 0,1 |
Chemikalien | 17 % Na2SO3, 3 % NaOH und 14 % Na2CO3 bezogen auf Holz |
0,07 % Anthrachinon während der Imprägnierung | |
10 v/v % Methanol in der Kochung, wird erst nach der Imprägnierung zugesetzt | |
Flotte | 3,3:1 (Flüssigkeit:Holz) während der Imprägnierung |
4:1 (Flüssigkeit:Holz) während des Aufschlusses | |
Technologie | Bereiten der Imprägnierlauge |
20 min Dämpfen des Aufschlußgutes | |
15 min Imprägnieren bei 122°C | |
10 min Methanoleingabe und LaugenLaugenverdrängung | |
60 min Aufheizen | |
200 min Fertigkochen bei 180°C | |
30 min Kochlauge verdrängen und Kocher entleeren | |
Ergebnis | Kappazahl: 19,8 |
Gutstoffausbeute: 50,8 % | |
Splitter 1,8 |
Claims (14)
- Sulfitaufschlußverfahren für lignozellulosehaltiges Rohmaterial unter Verwendung von wasserlöslichen alkalischen Monosulfitlösungen, organischen Lösungsmitteln sowie mindestens einem Chinonderivat, dadurch gekennzeichnet, daß das Rohmaterial vor dem eigentlichen Aufschluß des Rohmaterials einem Imprägnierungsschritt ohne organischen Lösungsmitteln in Anwesenheit der Monosulfitlösung und gegebenenfalls des Chinonderivats bei einer Temperatur, welche unterhalb der für die Aufschlußreaktion notwendige Temperatur liegt, unterzogen wird.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Rohmaterial während einer Zeitdauer von 5 bis 360 min, vorzugsweise von 15 bis 60 min, mit der Monosulfitlösung imprägniert wird.
- Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß das Rohmaterial bei einer Temperatur zwischen 60 und 150°C, vorzugsweise zwischen 100 und 130°C, mit der Monosulfitlösung imprägniert wird.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß eine Imprägnierlauge mit einer höheren Ionenstärke als die der Aufschlußlösung zum Einsatz kommt.
- Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß zur Beendigung des Imprägnierungsschrittes das organische Lösungsmittel oder das Lösungsmittel/Wasser-Gemisch in die Imprägnierlauge eingetragen wird.
- Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß die Ionenstärke der Imprägnierlauge durch den Eintrag des organischen Lösungsmittels oder des Lösungsmittel/Wasser-Gemisches auf die für den Aufschluß notwendige Konzentration eingestellt wird.
- Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß als organische Lösungsmittel ein- oder mehr wertige alkoholische Lösungsmittel, vorzugsweise Methanol, eingesetzt werden.
- Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß das Lösungsmittel während der Aufschlußreaktion in einer Menge zwischen 0,5 und 50 Volumenprozent der gesamten Flüssigkeitsmenge eingesetzt wird.
- Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß Natriumsulfit in den Monosulfitlösungen zum Einsatz kommt und zwar in einer Menge zwischen 5 und 40 % bezogen auf das Rohmaterial.
- Verfahren nach einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, daß wässerige Lösungen von Natriumhydroxid und/ oder Natriumkarbonat zu den Monosulfitlösungen gemischt werden und zwar in einer Menge zwischen 0 und 15 % bezogen auf das Rohmaterial.
- Verfahren nach einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, daß Kaliumhydroxid und/oder Kaliumcarbonat als Alkali in den Monosulfitlösungen zum Einsatz kommt.
- Verfahren nach einem der Ansprüche 1 bis 3 und 7 bis 11, dadurch gekennzeichnet, daß die Imprägnierlösung zur Beendigung des Imprägnierungsschrittes durch die Aufschlußlösung ersetzt wird .
- Verfahren nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, daß der Imprägnierungsschritt in diskontinuierlich arbeitenden Aufschlußsystemen durchgeführt wird, wobei die Imprägnierphase bereits in den Kochern durchgeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 13, dadurch gekennzeichnet, daß das Verfahren in kontinuierlich arbeitenden Aufschlußsystemen durchgeführt wird, wobei die Imprägnierphase in einem separaten Imprägnierturm (8) durchgeführt wird.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT0165194A AT401068B (de) | 1994-08-26 | 1994-08-26 | Sulfitaufschlussverfahren |
AT1651/94 | 1994-08-26 | ||
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 (de) |
CN (1) | CN1160426A (de) |
AT (2) | AT401068B (de) |
BR (1) | BR9508634A (de) |
CA (1) | CA2198485A1 (de) |
DE (1) | DE59504281D1 (de) |
ES (1) | ES2126305T3 (de) |
FI (1) | FI970707A0 (de) |
ID (1) | ID15812A (de) |
RU (1) | RU2124083C1 (de) |
WO (1) | WO1996006974A1 (de) |
ZA (1) | ZA956506B (de) |
Families Citing this family (3)
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 |
JP2012511918A (ja) * | 2008-12-17 | 2012-05-31 | ボレガード インダストリーズ リミテッド ノルゲ | リグノセルロース系バイオマス変換 |
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)
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)
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 |
-
1994
- 1994-08-26 AT AT0165194A patent/AT401068B/de not_active IP Right Cessation
-
1995
- 1995-08-03 ZA ZA956506A patent/ZA956506B/xx unknown
- 1995-08-25 DE DE59504281T patent/DE59504281D1/de not_active Expired - Fee Related
- 1995-08-25 CN CN95194771A patent/CN1160426A/zh active Pending
- 1995-08-25 CA CA002198485A patent/CA2198485A1/en not_active Abandoned
- 1995-08-25 RU RU97104473A patent/RU2124083C1/ru active
- 1995-08-25 ES ES95928394T patent/ES2126305T3/es not_active Expired - Lifetime
- 1995-08-25 EP EP95928394A patent/EP0777780B1/de not_active Expired - Lifetime
- 1995-08-25 BR BR9508634A patent/BR9508634A/pt not_active Application Discontinuation
- 1995-08-25 WO PCT/AT1995/000170 patent/WO1996006974A1/de active IP Right Grant
- 1995-08-25 AT AT95928394T patent/ATE173517T1/de not_active IP Right Cessation
- 1995-08-26 ID IDP951678A patent/ID15812A/id unknown
-
1997
- 1997-02-19 FI FI970707A patent/FI970707A0/fi unknown
Patent Citations (1)
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 |
CN1160426A (zh) | 1997-09-24 |
ID15812A (id) | 1997-08-14 |
ES2126305T3 (es) | 1999-03-16 |
ATA165194A (de) | 1995-10-15 |
BR9508634A (pt) | 1997-12-30 |
ATE173517T1 (de) | 1998-12-15 |
CA2198485A1 (en) | 1996-03-07 |
ZA956506B (en) | 1996-03-18 |
EP0777780A1 (de) | 1997-06-11 |
DE59504281D1 (de) | 1998-12-24 |
FI970707A (fi) | 1997-02-19 |
FI970707A0 (fi) | 1997-02-19 |
WO1996006974A1 (de) | 1996-03-07 |
AT401068B (de) | 1996-06-25 |
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