EP2148000A2 - Method for obtaining cellulose - Google Patents

Method for obtaining cellulose Download PDF

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Publication number
EP2148000A2
EP2148000A2 EP09009419A EP09009419A EP2148000A2 EP 2148000 A2 EP2148000 A2 EP 2148000A2 EP 09009419 A EP09009419 A EP 09009419A EP 09009419 A EP09009419 A EP 09009419A EP 2148000 A2 EP2148000 A2 EP 2148000A2
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EP
European Patent Office
Prior art keywords
segments
washing
raw materials
cellulose
screw
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EP09009419A
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German (de)
French (fr)
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EP2148000A3 (en
EP2148000B1 (en
Inventor
Oleg K. Nugmanov
Nadezhda P. Grigoriyeva
Nail I. Gainullin
Nikolai A. Lebedev
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OOO NPO "NEFTEPROMCHIM"
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OOO NPO 'Neftepromchim
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Priority to PL09009419T priority Critical patent/PL2148000T3/en
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00—Fibrous raw materials or their mechanical treatment
    • D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
    • D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
    • D21B1/30—Defibrating by other means
    • 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
    • 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
    • D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
    • 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
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse

Definitions

  • the invention relates to a process for obtaining cellulose comprising the following sequential steps: soaking the cellulosic raw materials from cabbage plants in an alkali solution, thermomechanical-chemical processing of the raw materials in a twin screw apparatus, comprising a heated chamber, 2 parallel coupled shafts installed inside the chamber where alternate auger segments and shredder cam segments are mounted, washing, bleaching, washing, skidding and drying.
  • the invention further relates to the cellulose industry and in particular the recovery of cellulose from vegetable cellulosic raw materials.
  • the invention can be used for the recovery of cellulose intended for petroleum processing, cotton wool production and the paper industry.
  • the Alkaliuf gleich is carried out at 120 - 130 ° C within 1 hour.
  • the liquor contains a surfactant.
  • the mass is then washed with a 1.5-fold amount of the clarified water, crushed and finely cleaned in a hydrocyclone with clarified water.
  • the twice bleaching with NaOCl solution is performed.
  • the temperature is 90 ° C
  • the pH is 9 - 11.5, the duration is 1 hour.
  • the following steps are carried out: washing with softened water, acidification with H 2 SO 4 solution at 15-40 ° C within 1 hour, repeated washing with softened water, spin-drying and air drying.
  • the temperature is 130-140 ° C
  • the pressure is 3-4 atm
  • the duration is 180-210 min. Further, the following steps are carried out: washing, bleaching with sodium hypochlorite in an acidic solution, spin-drying, loosening and drying ( RU 2078163 ).
  • a prototype is the process for obtaining cellulose from cellulosic raw materials by simultaneous loosening and cleaning steps and further successive steps: washing and comminution of the raw materials, soaking, thermomechanical-chemical processing, washing, bleaching, washing, ejection and drying.
  • the raw materials are allowed to mature in an alkali solution ( RU 2007115321 ).
  • the invention is based on the object to provide an efficient and cost-effective method for the production of cellulose from cellulose-containing raw materials available.
  • raw materials herbaceous plants, in particular with a high content of shives, the woody inner part and lignin, with a large deposit duration on the fields and in storage rooms, can be used.
  • Two parallel coupled shafts are installed in a heated chamber. Alternate auger and crushing cam segments are mounted on the shafts.
  • thermo-mechanical-chemical processing is carried out before washing in a twin-screw apparatus, on the shafts of which alternating conveyor and brake screw segments are mounted.
  • cellulose-containing raw materials are preferably herbaceous plants, such as fiber flax, L. subsp. intermedium, oil flax, green flax, oilseed rape, miscanthus, clover, alfalfa, caster, Jerusalem artichoke, galega, Heracleum sosnowskyi, corn, etc., in various degrees of maturity, with high content of woody interior and lignin and with a large deposit duration, for example, in the fields and used in storage rooms.
  • herbaceous plants such as fiber flax, L. subsp. intermedium, oil flax, green flax, oilseed rape, miscanthus, clover, alfalfa, caster, Jerusalem artichoke, galega, Heracleum sosnowskyi, corn, etc.
  • the twin screw apparatus comprises a working chamber with a dense wall, feed and drainage nozzles. Within the working chamber two parallel coupled shafts can be installed. Attachments of various purpose may be mounted on the shafts: augers, crushing cam and brake screw segments. The worm segments can be mounted alternately on the shafts. (Copyright of the USSR No. 884715 . 1981 ).
  • the working chamber is favorably equipped with resistance heating elements.
  • the heating elements can be laid around the outside of the wall. All heating elements can be connected to a controlled external power source.
  • a thermosensor can be connected to the control input of this power source.
  • cellulosic raw materials in particular the aforementioned from herbaceous plants, are pre-soaked in an alkali solution.
  • the solution can be prepared with circulating water having a NaOH content of 10 to 60 g / l and a surfactant content of 0.2 to 0.8 g / l.
  • the soaking can be done at 90-100 ° C for 15-60 minutes.
  • the hydraulic modulus (the ratio of the solid / liquid phases) can be 1: (10 + 20).
  • the heated pulp with 5 - 10% of the cellulosic raw materials is then conveniently in the on z. B. 80 -100 ° C heated twin screw apparatus.
  • alternating auger, crushing cam and brake screw segments may be mounted on the shafts of the twin screw apparatus.
  • the screw segments can be displaced relative to one another such that a screw channel is formed.
  • the turns of the screw segments can have the same diameter, the same direction and a fixed gear per screw segment.
  • the winding path of each next screw segment may be smaller than the winding path of the previous screw segment.
  • the distance between the turns of the screw segments and the inner wall of the working chamber may be 0.5 - 10 mm.
  • the direction of the screw channel of the shredding cam segments and the direction of the screw flights may coincide.
  • Preferably 10-16 screw conveyor segments and 5-20 crushing cam segments are used.
  • the processed pulp is in the z. B. 85 - 105 ° C heated twin screw apparatus transported.
  • Alternating conveyor and brake screw segments can be mounted on the shafts of the apparatus.
  • the screw conveyor segments may have 2 (or more) turns more than brake screw segments.
  • thermomechanical-chemical processing is carried out before washing.
  • the processed pulp is conveyed to the twin screw apparatus heated to, for example, 90-110 ° C.
  • alternating auger, crushing cam and brake screw segments may be mounted on the shafts of the apparatus.
  • Preferably 10 to 16 screw conveyor segments are used, preferably 7 to 20 crushing cam segments and preferably 4 to 10 brake screw segments.
  • the pulp may be washed in softened water to remove the alkali radicals from the cellulosic mass.
  • the washing is conveniently carried out in two stages.
  • the mass is allowed in containers filled with water within z. B. 20 - 30 minutes at z. B. 80 - 90 ° C and within z. B. 20 - 30 minutes at z. B. 40 - 50 ° C lie.
  • the hydraulic module can be used at any level 1: (10 20).
  • the bleaching of the flax cellulose can be carried out in a hydrogen peroxide solution having a concentration of e.g. B. 5 - 10 g / l at conveniently 85 - 95 ° C within z. B. 90 minutes.
  • the hydraulic module can be 1: (10 20).
  • the cellulose is further washed with softened water, for example, as well as after Alkaliuf gleich.
  • the centrifuging can be carried out in centrifuges of type AG or AOG up to z. B. 40 - 50% moisture.
  • the cellulose can be dried, for example, with combustion gases at 140-160 ° C in a Vibrotrockner.
  • the dried cellulose can be carried in a cyclone for air separation and on to the packaging.
  • Two parallel coupled shafts are installed in a heated chamber. Alternate auger and crushing cam segments are mounted on the shafts.
  • thermo-mechanical-chemical processing is carried out before washing in a twin-screw apparatus, on the shafts of which alternating conveyor and brake screw segments are mounted.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

Process for extracting cellulose comprises soaking the cellulose containing raw materials from herbaceous plants in an alkaline solution, thermomechanical-chemical processing of raw materials in a twin-screw apparatus comprising a heated chamber, two parallely coupled shaft installed within the chamber, on which alternating screw conveyor segments and grinding cam segments are mounted, washing, bleaching, again washing, centrifuging and drying, where before washing, an additional thermo-chemical processing in a twin-screw apparatus, is carried out. Process for extracting cellulose comprises soaking the cellulose containing raw materials from herbaceous plants in an alkaline solution, thermomechanical-chemical processing of raw materials in a twin-screw apparatus comprising a heated chamber, two parallely coupled shaft installed within the chamber, on which alternative screw conveyor segments and grinding cam segments are mounted, washing, bleaching, again washing, centrifuging and drying, where before washing, an additional thermo-chemical processing in a twin-screw apparatus, on which shaft of alternative screw conveyor segments and brake screw segments are mounted, is carried out.

Description

Die Erfindung betrifft ein Verfahren zur Gewinnung von Cellulose mit folgenden aufeinanderfolgenden Schritten: Einweichen der cellulosehaltigen Rohstoffe aus Krautpflanzen in einer Alkalilösung, thermomechanisch-chemisches Verarbeiten der Rohstoffe in einem Doppelschneckenapparat, umfassend eine beheizte Kammer, 2 innerhalb der Kammer installierte, parallel gekoppelte Wellen, auf denen alternierende Förderschneckensegmente und Zerkleinerungsnockensegmente montiert sind, Waschen, Bleichen, Waschen, Ausschleudern und Trocknen.The invention relates to a process for obtaining cellulose comprising the following sequential steps: soaking the cellulosic raw materials from cabbage plants in an alkali solution, thermomechanical-chemical processing of the raw materials in a twin screw apparatus, comprising a heated chamber, 2 parallel coupled shafts installed inside the chamber where alternate auger segments and shredder cam segments are mounted, washing, bleaching, washing, skidding and drying.

Die Erfindung betrifft ferner die Celluloseindustrie und insbesondere die Gewinnung von Cellulose aus pflanzlichen cellulosehaltigen Rohstoffen. Die Erfindung kann für die Gewinnung von Cellulose, die für die Erdölverarbeitung, die Watteproduktion und die Papierindustrie bestimmt ist, eingesetzt werden.The invention further relates to the cellulose industry and in particular the recovery of cellulose from vegetable cellulosic raw materials. The invention can be used for the recovery of cellulose intended for petroleum processing, cotton wool production and the paper industry.

Bekannt ist ein Verfahren zur Gewinnung von Cellulose, das Lockern der Rohstoffe und Alkaliaufschluss einschließt. Der Alkaliaufschluss wird bei 120 - 130 °C innerhalb von 1 Stunde durchgeführt. Die Lauge enthält dabei ein Tensid. Die Masse wird danach mit einer 1,5-fachen Menge des geklärten Wassers gewaschen, zerkleinert und in einem Hydrozyklon mit geklärtem Wasser feingereinigt. Dann wird das zweimalige Bleichen mit NaOCl-Lösung durchgeführt. Die Temperatur beträgt 90 °C, der pH-Wert liegt bei 9 - 11,5, die Dauer ist 1 Stunde. Danach werden folgende Schritte durchgeführt: Waschen mit enthärtetem Wasser, Absäuern mit H2SO4-Lösung bei 15 - 40 °C innerhalb von 1 Stunde, nochmaliges Waschen mit enthärtetem Wasser, Ausschleudern und Lufttrocknen.Known is a process for the recovery of cellulose, which includes loosening the raw materials and alkali digestion. The Alkaliufschluss is carried out at 120 - 130 ° C within 1 hour. The liquor contains a surfactant. The mass is then washed with a 1.5-fold amount of the clarified water, crushed and finely cleaned in a hydrocyclone with clarified water. Then the twice bleaching with NaOCl solution is performed. The temperature is 90 ° C, the pH is 9 - 11.5, the duration is 1 hour. Thereafter, the following steps are carried out: washing with softened water, acidification with H 2 SO 4 solution at 15-40 ° C within 1 hour, repeated washing with softened water, spin-drying and air drying.

Bekannt ist ferner ein Verfahren zur Gewinnung von Cellulose, das die mechanische Verarbeitung der cellulosehaltigen Rohstoffe durch gleichzeitige Lockern- und Reinigungsstufen einschließt. Danach erfolgt Alkaliaufschluss. Die Temperatur beträgt dabei 130 - 140 °C, der Druck ist 3 - 4 Atm, die Dauer ist 180 - 210 Min. Weiter werden folgende Schritte durchgeführt: Waschen, Bleichen mit Natriumhypochlorit in einer sauren Lösung, Ausschleudern, Lockern und Trocknen ( RU 2078163 ).Also known is a process for the production of cellulose, which includes the mechanical processing of cellulose-containing raw materials by simultaneous loosening and purification steps. Thereafter, alkali entrapment takes place. The temperature is 130-140 ° C, the pressure is 3-4 atm, the duration is 180-210 min. Further, the following steps are carried out: washing, bleaching with sodium hypochlorite in an acidic solution, spin-drying, loosening and drying ( RU 2078163 ).

Des Weiteren ist ein Verfahren zur Gewinnung von Cellulose aus cellulosehaltigen Rohstoffen durch gleichzeitige Lockern- und Reinigungsstufen und nachfolgende Zerkleinerung, Einweichen in einer Alkalilösung und Reinigung bekannt. Danach erfolgt Alkaliaufschluss im Laufe von 1,5 - 3 Stunden beim hydraulischen Modul (Verhältnis der festen/flüssigen Phasen) von 1:(5-20). Zusätzlich wird in die Lauge ein Tensid zugegeben. Danach erfolgen Waschen, Bleichen in der Wasserstoffperoxidlösung, nochmaliges Waschen, Ausschleudern und Trocknen ( RU 2304647 ).Furthermore, a process for the recovery of cellulose from cellulosic raw materials by simultaneous loosening and purification steps and subsequent comminution, soaking in an alkali solution and purification is known. Thereafter, alkali fusion occurs in the course of 1.5-3 hours with the hydraulic modulus (ratio of solid / liquid phases) of 1: (5-20). In addition, a surfactant is added to the liquor. This is followed by washing, bleaching in the hydrogen peroxide solution, repeated washing, ejection and drying ( RU 2304647 ).

Als Prototyp dient das Verfahren zur Gewinnung von Cellulose aus cellulosehaltigen Rohstoffen durch gleichzeitige Lockern- und Reinigungsstufen und weitere aufeinander folgende Schritte: Waschen und Zerkleinerung der Rohstoffe, Einweichen, thermomechanisch-chemische Verarbeitung, Waschen, Bleichen, Waschen, Ausschleudern und Trocknen. In einer Ausführungsvariante des Verfahrens lässt man die Rohstoffe in einer Alkalilösung ausreifen ( RU 2007115321 ).A prototype is the process for obtaining cellulose from cellulosic raw materials by simultaneous loosening and cleaning steps and further successive steps: washing and comminution of the raw materials, soaking, thermomechanical-chemical processing, washing, bleaching, washing, ejection and drying. In one embodiment of the process, the raw materials are allowed to mature in an alkali solution ( RU 2007115321 ).

Der Erfindung liegt die Aufgabe zu Grunde, ein effizientes und kostengünstiges Verfahren zur Gewinnung von Cellulose aus cellulosehaltigen Rohstoffen zur Verfügung zu stellen. Als Rohstoffe können Krautpflanzen insbesondere mit hohem Gehalt an Schäben, dem holzigen Innenteil und Lignin, mit großer Ablagerungsdauer auf den Feldern und in Lagerräumen, eingesetzt werden.The invention is based on the object to provide an efficient and cost-effective method for the production of cellulose from cellulose-containing raw materials available. As raw materials, herbaceous plants, in particular with a high content of shives, the woody inner part and lignin, with a large deposit duration on the fields and in storage rooms, can be used.

Die gestellte Aufgabe wird durch die Merkmale des Anspruch 1 gelöst. Dabei sind folgende Stufen vorgesehen:

  1. a) Einweichen der cellulosehaltigen Rohstoffe in einer Alkalilösung;
  2. b) thermomechanisch-chemische Verarbeitung in einem Doppelschneckenapparat;
  3. c) Waschen, Bleichen, Waschen, Ausschleudern und Trocknen.
The stated object is solved by the features of claim 1. The following stages are provided:
  1. a) soaking the cellulose-containing raw materials in an alkali solution;
  2. b) thermomechanical-chemical processing in a twin screw apparatus;
  3. c) washing, bleaching, washing, spin-drying and drying.

Der Doppelschneckenapparat umfasst:

  1. a) eine beheizte Kammer;
  2. b) 2 parallel gekoppelte Wellen;
  3. c) Förderschneckensegmente;
  4. d) Zerkleinerungsnockensegmente.
The twin screw apparatus includes:
  1. a) a heated chamber;
  2. b) 2 parallel coupled waves;
  3. c) screw conveyor segments;
  4. d) shredding cam segments.

Die einzelnen Elemente sowie ihre funktionelle Verbindung zum Doppelschneckenapparat, wie er im erfindungsgemäßen Verfahren eingesetzt wird, sind dem Fachmann an sich bekannt.The individual elements and their functional connection to the twin-screw apparatus, as used in the process according to the invention, are known per se to the person skilled in the art.

Zwei parallel gekoppelte Wellen sind in einer beheizten Kammer installiert. Auf den Wellen sind alternierende Förderschnecken- und Zerkleinerungsnockensegmente montiert.Two parallel coupled shafts are installed in a heated chamber. Alternate auger and crushing cam segments are mounted on the shafts.

Die zusätzliche thermomechanisch-chemische Verarbeitung wird vor dem Waschen in einem Doppelschneckenapparat, auf dessen Wellen alternierende Förder- und Bremsschneckensegmente montiert sind, durchgeführt.The additional thermo-mechanical-chemical processing is carried out before washing in a twin-screw apparatus, on the shafts of which alternating conveyor and brake screw segments are mounted.

Es ist möglich, alternierende Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente auf die Wellen zu montieren.It is possible to mount alternating augers, crushing cam and brake screw segments on the shafts.

Als cellulosehaltige Rohstoffe werden vorzugsweise Krautpflanzen, beispielsweise Faserfflachs, L. subsp. intermedium, Ölflachs, Grünflachs, Raps, Miscanthus, Steinklee, Luzerne, Rizinusstaude, Topinambur, Galega, Heracleum sosnowskyi, Mais usw., in verschiedenen Ausreifungsgraden, mit hohem Gehalt am holzigen Innenteil und Lignin und mit einer großen Ablagerungsdauer bspw. auf den Feldern und in Lagerräumen eingesetzt.As cellulose-containing raw materials are preferably herbaceous plants, such as fiber flax, L. subsp. intermedium, oil flax, green flax, oilseed rape, miscanthus, clover, alfalfa, caster, Jerusalem artichoke, galega, Heracleum sosnowskyi, corn, etc., in various degrees of maturity, with high content of woody interior and lignin and with a large deposit duration, for example, in the fields and used in storage rooms.

Der Doppelschneckenapparat umfasst eine Arbeitskammer mit einer dichten Wand, Beschickungs- und Entleerungsstutzen. Innerhalb der Arbeitskammer können zwei parallel gekoppelte Wellen installiert sein. Auf den Wellen können Aufsatzstücke verschiedener Zweckbestimmung montiert sein: Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente. Die Schneckensegmente können auf den Wellen alternierend montiert sein. (Urheberschein der UdSSR No. 884715 , 1981 ).The twin screw apparatus comprises a working chamber with a dense wall, feed and drainage nozzles. Within the working chamber two parallel coupled shafts can be installed. Attachments of various purpose may be mounted on the shafts: augers, crushing cam and brake screw segments. The worm segments can be mounted alternately on the shafts. (Copyright of the USSR No. 884715 . 1981 ).

Im erfindungsgemäßen Verfahren ist die Arbeitskammer günstigerweise mit Widerstandsheizelementen ausgestattet. Die Heizelemente können außen um die Wand herum verlegt sein. Alle Heizelemente können an eine gesteuerte Außenstromquelle angeschlossen sein. An den Steuereingang dieser Stromquelle kann ein Thermosensor angeschlossen sein.In the method according to the invention, the working chamber is favorably equipped with resistance heating elements. The heating elements can be laid around the outside of the wall. All heating elements can be connected to a controlled external power source. A thermosensor can be connected to the control input of this power source.

Im erfindungsgemäßen Verfahren werden cellulosehaltige Rohstoffe insbesondere die vorgenannten aus Krautpflanzen, in einer Alkalilösung voreingeweicht. Die Lösung kann mit Kreislaufwasser mit einem NaOH-Gehalt von 10 - 60 g/l und einem Tensidgehalt von 0,2 - 0,8 g/l zubereitet sein. Das Einweichen kann während 15 - 60 Minuten bei 90 -100 °C erfolgen. Das hydraulische Modul (das Verhältnis der festen/flüssigen Phasen) kann 1:(10+20) betragen.In the process according to the invention, cellulosic raw materials, in particular the aforementioned from herbaceous plants, are pre-soaked in an alkali solution. The solution can be prepared with circulating water having a NaOH content of 10 to 60 g / l and a surfactant content of 0.2 to 0.8 g / l. The soaking can be done at 90-100 ° C for 15-60 minutes. The hydraulic modulus (the ratio of the solid / liquid phases) can be 1: (10 + 20).

Die geheizte Pulpe mit 5 - 10 % der cellulosehaltigen Rohstoffe wird danach günstigerweise in den auf z. B. 80 -100 °C geheizten Doppelschneckenapparat befördert. Auf den Wellen des Doppelschneckenapparates können alternierende Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente montiert sein. Die Schneckensegmente können so zueinander verschoben sein, dass ein Schraubenkanal gebildet wird.The heated pulp with 5 - 10% of the cellulosic raw materials is then conveniently in the on z. B. 80 -100 ° C heated twin screw apparatus. On the shafts of the twin screw apparatus alternating auger, crushing cam and brake screw segments may be mounted. The screw segments can be displaced relative to one another such that a screw channel is formed.

Die Windungen der Schneckensegmente können einen gleichen Durchmesser, eine gleiche Richtung und einen festen Gang je Schneckensegment aufweisen. Der Windungsgang jedes nächsten Schneckensegmentes kann kleiner als der Windungsgang des vorherigen Schneckensegmentes sein. Der Abstand zwischen den Windungen der Schneckensegmente und der Innenwand der Arbeitskammer kann 0,5 - 10 mm betragen. Die Richtung des Schraubenkanals der Zerkleinerungsnockensegmente und die Richtung der Schneckenwindungen können übereinstimmen. Es werden vorzugsweise 10 - 16 Förderschneckensegmente und 5 - 20 Zerkleinerungsnockensegmente eingesetzt.The turns of the screw segments can have the same diameter, the same direction and a fixed gear per screw segment. The winding path of each next screw segment may be smaller than the winding path of the previous screw segment. The distance between the turns of the screw segments and the inner wall of the working chamber may be 0.5 - 10 mm. The direction of the screw channel of the shredding cam segments and the direction of the screw flights may coincide. Preferably 10-16 screw conveyor segments and 5-20 crushing cam segments are used.

Die verarbeitete Pulpe wird in den auf z. B. 85 - 105 °C erhitzten Doppelschneckenapparat befördert. Auf den Wellen des Apparates können alternierende Förder- und Bremsschneckensegmente montiert sein. Die Förderschneckensegmente können 2 (oder mehr) Windungen mehr als Bremsschneckensegmente aufweisen.The processed pulp is in the z. B. 85 - 105 ° C heated twin screw apparatus transported. Alternating conveyor and brake screw segments can be mounted on the shafts of the apparatus. The screw conveyor segments may have 2 (or more) turns more than brake screw segments.

Wenn cellulosehaltige Rohstoffe spätreif sind, lange in Lagerräumen oder auf den Feldern abgelagert wurden oder einen hohen Ligningehalt haben, wird eine zusätzliche thermomechanisch-chemische Verarbeitung vor dem Waschen durchgeführt. Die verarbeitete Pulpe wird in den auf beispielsweise 90 - 110 °C erhitzten Doppelschneckenapparat befördert. Auf den Wellen des Apparates können alternierende Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente montiert sein. Es werden vorzugsweise 10 - 16 Förderschneckensegmente, vorzugsweise 7 - 20 Zerkleinerungsnockensegmente und vorzugsweise 4 - 10 Bremsschneckensegmente eingesetzt.If cellulosic raw materials are late-ripened, have been stored for a long time in storerooms or on the fields or have a high lignin content, additional thermomechanical-chemical processing is carried out before washing. The processed pulp is conveyed to the twin screw apparatus heated to, for example, 90-110 ° C. On the shafts of the apparatus, alternating auger, crushing cam and brake screw segments may be mounted. Preferably 10 to 16 screw conveyor segments are used, preferably 7 to 20 crushing cam segments and preferably 4 to 10 brake screw segments.

Die Pulpe kann in enthärtetem Wasser zur Entfernung der Alkalireste aus der Cellulosemasse gewaschen werden. Das Waschen erfolgt günstigerweise in zwei Stufen. Die Masse lässt man in mit Wasser befüllten Behältern innerhalb von z. B. 20 - 30 Minuten bei z. B. 80 - 90 °C und innerhalb von z. B. 20 - 30 Minuten bei z. B. 40 - 50 °C liegen. Das hydraulische Modul kann auf jeder Stufe 1:(10

Figure imgb0001
20) betragen.The pulp may be washed in softened water to remove the alkali radicals from the cellulosic mass. The washing is conveniently carried out in two stages. The mass is allowed in containers filled with water within z. B. 20 - 30 minutes at z. B. 80 - 90 ° C and within z. B. 20 - 30 minutes at z. B. 40 - 50 ° C lie. The hydraulic module can be used at any level 1: (10
Figure imgb0001
20).

Das Bleichen der Flachscellulose kann in einer Wasserstoffperoxidlösung mit einer Konzentration von z. B. 5 - 10 g/l bei günstigerweise 85 - 95 °C innerhalb von z. B. 90 Minuten. Das hydraulische Modul kann 1:(10

Figure imgb0002
20) betragen.The bleaching of the flax cellulose can be carried out in a hydrogen peroxide solution having a concentration of e.g. B. 5 - 10 g / l at conveniently 85 - 95 ° C within z. B. 90 minutes. The hydraulic module can be 1: (10
Figure imgb0002
20).

Die Cellulose wird weiter mit enthärtetem Wasser gewaschen, bspw. genauso wie nach dem Alkaliaufschluss.The cellulose is further washed with softened water, for example, as well as after Alkaliufschluss.

Das Ausschleudern kann in Zentrifugen vom Typ AG oder AOG bis z. B. 40 - 50 % Feuchtigkeit erfolgen.The centrifuging can be carried out in centrifuges of type AG or AOG up to z. B. 40 - 50% moisture.

Die Cellulose kann bspw. mit Verbrennungsgasen bei 140 -160 °C in einem Vibrotrockner getrocknet werden.The cellulose can be dried, for example, with combustion gases at 140-160 ° C in a Vibrotrockner.

Die getrocknete Cellulose kann in einem Zyklon für die Luftabtrennung und weiter zur Verpackung befördert werden.The dried cellulose can be carried in a cyclone for air separation and on to the packaging.

In der nachfolgenden Tabelle sind Ausführungsbeispiele 1 - 13 gemäß dem erfindungsgemäßen Verfahren aufgeführt.The following table shows exemplary embodiments 1-13 according to the method according to the invention.

Die Qualität der gewonnenen Cellulose wird entsprechend GOST 595-79 "Baumwollcellulose" geprüft. Physikalisch-chemische Kenndaten der gewonnenen Cellulose sind in der Tabelle zusammengefasst.The quality of the recovered cellulose is tested according to GOST 595-79 "Cotton Cellulose". Physicochemical characteristics of the recovered cellulose are summarized in the table.

Das Verfahren ist effizient. Es gestattet, Cellulose aus Krautpflanzen mit einer hohen Ertragsfähigkeit und einem hohen wirtschaftlichen Anbaupotential zu gewinnen. Selbstkosten der Cellulose sind wesentlich niedriger, d. h. die Cellulose kann mit dem erfindungsgemäßen Verfahren überraschenderweise sehr kostengünstig hergestellt werden. Tabelle Beispiel Verarbeitete cellulose-haltige Rohstoffe Physikalisch - chemische Kenndaten der Cellulose Massenanteil an α-Cellulose, % Massenan teil an Asche, % Massenanteil an Harze und Fette, % Rohstoffe mit einem mittleren Reifegrad Nach Anspruch 1 1. Faserflachs 96,4 0,05 0,11 2. Steinklee 92,7 0,3 0,05 3. Heracleum sosnowskyi 91,9 0,32 0,04 4. Galega 95,8 0,09 0,07 5. Luzerne 91,5 0,27 0,05 6. Topinambur 93,4 0,21 0,14 Rohstoffe mit einer hohen Ablagerungs dauer auf Feldern Nach Ansprüchen 1, 2 7. Rizinusstaude 96,2 0,39 0,09 8. Raps 95,6 0,13 0,06 9. Ölflachs 94,4 0,21 0,31 Rohstoffe mit einer hohen Ablagerungs dauer in Lagerräumen Nach Ansprüchen 1, 2 10. Stroh von Linum subsp. intermedium 96,1 0,15 0,26 11. Mais 94,4 0,18 0,12 12. Topinambur 93,6 0,22 0,04 13. Faserflachsstroh 95,9 0,14 0,20 14. Prototyp 91 0,41 0,20 The process is efficient. It makes it possible to obtain cellulose from herbaceous plants with a high yield and a high economic growing potential. Cost of the cellulose are substantially lower, that is, the cellulose can surprisingly be produced very inexpensively with the inventive method surprisingly. table example Processed cellulose-containing raw materials Physicochemical characteristics of cellulose Mass fraction of α-cellulose,% Mass fraction of ash,% Mass fraction of resins and fats,% Raw materials with a medium degree of ripeness According to claim 1 1. flax 96.4 0.05 0.11 Second sweet clover 92.7 0.3 0.05 Third Heracleum sosnowskyi 91.9 0.32 0.04 4th Galega 95.8 0.09 0.07 5th alfalfa 91.5 0.27 0.05 6th Jerusalem artichokes 93.4 0.21 0.14 Raw materials with a high deposit duration on fields According to claims 1, 2 7th gourd 96.2 0.39 0.09 8th. rape 95.6 0.13 0.06 9th oil flax 94.4 0.21 0.31 Raw materials with a high deposit duration in storage rooms According to claims 1, 2 10th Straw from Linum subsp. intermedium 96.1 0.15 0.26 11th Corn 94.4 0.18 0.12 12th Jerusalem artichokes 93.6 0.22 0.04 13th Fiber flax straw 95.9 0.14 0.20 14th prototype 91 0.41 0.20

Fragment der AnmeldungFragment of the application

Das Verfahren zur Gewinnung der Cellulose umfasst:

  1. a) Einweichen der cellulosehaltigen Rohstoffe in einer Alkalilösung;
  2. b) thermomechanisch-chemische Verarbeitung in einem Doppelschneckenapparat;
  3. c) Waschen, Bleichen, Waschen, Ausschleudern, Trocknen.
The process for recovering the cellulose comprises:
  1. a) soaking the cellulose-containing raw materials in an alkali solution;
  2. b) thermomechanical-chemical processing in a twin screw apparatus;
  3. c) washing, bleaching, washing, spin-drying, drying.

Der Doppelschneckenapparat umfasst:

  1. a) einer beheizten Kammer,
  2. b) 2 parallel gekoppelten Wellen;
  3. c) Förderschneckensegmenten;
  4. d) Zerkleinerungsnockensegmenten.
The twin screw apparatus includes:
  1. a) a heated chamber,
  2. b) 2 parallel coupled waves;
  3. c) screw conveyor segments;
  4. d) shredding cam segments.

Zwei parallel gekoppelte Wellen sind in einer beheizten Kammer installiert. Auf den Wellen sind alternierende Förderschnecken- und Zerkleinerungsnockensegmente montiert.Two parallel coupled shafts are installed in a heated chamber. Alternate auger and crushing cam segments are mounted on the shafts.

Die zusätzliche thermomechanisch-chemische Verarbeitung wird vor dem Waschen in einem Doppelschneckenapparat, auf dessen Wellen alternierende Förder- und Bremsschneckensegmente montiert sind, durchgeführt.The additional thermo-mechanical-chemical processing is carried out before washing in a twin-screw apparatus, on the shafts of which alternating conveyor and brake screw segments are mounted.

Es ist möglich, alternierende Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente auf die Wellen zu montieren.It is possible to mount alternating augers, crushing cam and brake screw segments on the shafts.

Claims (2)

Verfahren zur Gewinnung von Cellulose mit folgenden aufeinanderfolgenden Schritten: Einweichen der cellulosehaltigen Rohstoffe aus Krautpflanzen in einer Alkalilösung, thermomechanisch-chemisches Verarbeiten der Rohstoffe in einem Doppelschneckenapparat, umfassend eine beheizte Kammer, 2 innerhalb der Kammer installierte, parallel gekoppelte Wellen, auf denen alternierende Förderschneckensegmente und Zerkleinerungsnockensegmente montiert sind, Waschen, Bleichen, Waschen, Ausschleudern und Trocknen,
dadurch gekennzeichnet,
dass vor dem Waschen eine zusätzliche thermomechanisch-chemische Verarbeitung in einem Doppelschneckenapparat, auf dessen Wellen alternierende Förder- und Bremsschneckensegmente montiert sind, durchgeführt wird.Process for the recovery of cellulose comprising the following sequential steps: soaking the cellulosic raw materials from herbaceous plants in an alkaline solution, thermomechanical-chemical processing of the raw materials in a twin screw apparatus comprising a heated chamber, 2 parallel coupled shafts installed inside the chamber, on which alternate auger segments and Crushing cam segments are mounted, washing, bleaching, washing, ejecting and drying,
characterized,
that an additional thermo-mechanical chemical processing in a twin screw apparatus, alternating conveying and braking screw segments are mounted on the shafts, is performed before washing. Verfahren nach Anspruch 1,
dadurch gekennzeichnet,
dass vor dem Waschen eine zusätzliche thermomechanisch-chemische Verarbeitung in einem Doppelschneckenapparat, auf dessen Wellen alternierende Förderschnecken-, Zerkleinerungsnocken- und Bremsschneckensegmente montiert sind, durchgeführt wird.Method according to claim 1,
characterized,
that an additional thermo-mechanical chemical processing in a twin screw apparatus, alternating auger, Zerkleinerungsnocken- and braking screw segments are mounted on the shafts, is performed before washing.
EP20090009419 2008-07-24 2009-07-21 Method for obtaining cellulose Not-in-force EP2148000B1 (en)

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CN103317572A (en) * 2013-05-29 2013-09-25 台州金晟环保制品有限公司 Dry-process molding product bamboo fiber manufacturing method
CN103450363A (en) * 2013-08-12 2013-12-18 山东理工大学 Method for combined extraction of ginger starch and cellulose
CN105625074A (en) * 2016-02-24 2016-06-01 张民贵 Process for preparing pulp from hemp stems
CN108130771A (en) * 2017-12-08 2018-06-08 齐鲁工业大学 Clean pulping catalyst and its technique for applying
RU2761239C1 (en) * 2021-06-21 2021-12-06 федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский университет ИТМО» (Университет ИТМО) Method for producing cellulose

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RU2566275C1 (en) * 2014-07-24 2015-10-20 Федеральное государственное бюджетное учреждение науки Институт проблем химико-энергетических технологий Сибирского отделения РАН (ИПХЭТ СО РАН) Method of obtaining of cellulose from half-wit flax for paper industry
CN111570474A (en) * 2020-05-18 2020-08-25 长沙季丰科技有限公司 Environment-friendly treatment and recycling method of areca residue

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CN103317572A (en) * 2013-05-29 2013-09-25 台州金晟环保制品有限公司 Dry-process molding product bamboo fiber manufacturing method
CN103450363A (en) * 2013-08-12 2013-12-18 山东理工大学 Method for combined extraction of ginger starch and cellulose
CN103450363B (en) * 2013-08-12 2016-01-27 山东理工大学 A kind of combined extracting ginger starch, cellulosic method
CN105625074A (en) * 2016-02-24 2016-06-01 张民贵 Process for preparing pulp from hemp stems
CN108130771A (en) * 2017-12-08 2018-06-08 齐鲁工业大学 Clean pulping catalyst and its technique for applying
RU2761239C1 (en) * 2021-06-21 2021-12-06 федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский университет ИТМО» (Университет ИТМО) Method for producing cellulose

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