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EP0861347A1 - Method of obtaining cellulose fibre material from a plant substrate containing calcium pectinate - Google Patents

Method of obtaining cellulose fibre material from a plant substrate containing calcium pectinate

Info

Publication number
EP0861347A1
EP0861347A1 EP95940192A EP95940192A EP0861347A1 EP 0861347 A1 EP0861347 A1 EP 0861347A1 EP 95940192 A EP95940192 A EP 95940192A EP 95940192 A EP95940192 A EP 95940192A EP 0861347 A1 EP0861347 A1 EP 0861347A1
Authority
EP
European Patent Office
Prior art keywords
solution
water
borax
per liter
amount
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.)
Granted
Application number
EP95940192A
Other languages
German (de)
French (fr)
Other versions
EP0861347B1 (en
Inventor
Herbert Costard
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.)
Windi Winderlich GmbH
Original Assignee
Windi Winderlich GmbH
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Filing date
Publication date
Application filed by Windi Winderlich GmbH filed Critical Windi Winderlich GmbH
Publication of EP0861347A1 publication Critical patent/EP0861347A1/en
Application granted granted Critical
Publication of EP0861347B1 publication Critical patent/EP0861347B1/en
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
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • 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
    • D21C3/006—Pulping cellulose-containing materials with compounds not otherwise provided for

Definitions

  • the invention relates to a process for the production of cellulose fiber material from vegetable substrate containing calcium pectinate.
  • Vegetable substrates have been used for a long time for the production of cellulose fiber materials.
  • a material is, for example, cellulose, which is generally obtained from wood and is an important commercial product that is used for paper production.
  • the class of cellulose fibers also includes so-called sclerenchyma or bast fibers, which form the supporting tissue of plants such as stalks or stems. In nature, these fibers are always in combination with substances such as lignins and pectins. These accompanying substances must be removed if the cellulose fiber material is to be obtained in a form suitable for further processing.
  • the plant substrate used is digested, de-wooded, de-pectinized and, if necessary, also bleached.
  • the raw material is the most important and currently used on a technical scale for cellulose production digested with sodium hydroxide solution.
  • Different additional chemicals can be present here.
  • sodium digestion NaOH, Na 2 CO 3
  • the sulfide process CaO, MgO, NaOH, NH 4 OH / SO 2
  • the sulfate process NaOH, Na 2 S, Na 2 CO 3
  • the chemicals mentioned each form the so-called "cooking acids”.
  • the digestion primarily results in the delignification (de-lignification) of the plant substrate, the lignins contained in the substrate being converted into a soluble form.
  • the known methods have the disadvantage that, in addition to the desired delignification, the cellulose fibers are also attacked to a considerable extent. This means that the strength of the pulp obtained at the end is reduced. The cellulose yield also drops. Therefore, not only is the lignin dissolved, but also some of the cellulose fibers of interest are undesirably destroyed. It is believed that the degree of polymerization is reduced or the fiber length is shortened. Some of the cellulose even goes into solution.
  • the known digestion processes also cause problems due to the waste products to be disposed of, the waste water question in particular being an important aspect.
  • the pectins and calcium pectinates present in the plant substrates must also be removed, the calcium pectinates in particular generally causing difficulties.
  • the invention is therefore based on the object of providing a new process for the production of cellulose fiber material from plant substrate containing calcium pectinate, in which the cellulose fibers are not damaged, compared to the known processes the environment less burdened and the duration of the procedure can be shortened.
  • This object is achieved by a process in which the vegetable substrate is digested and optionally bleached, the process being characterized in that trisodium phosphate is used for the digesting.
  • Trisodium phosphate is usually used for softening water such as boiler feed water, for phosphating, as a component of soap powders and toilet soaps, in dishwashing detergents or as a buffer.
  • the vegetable substrate used in the claimed process is preferably selected from plants of the Linaceae, Urticaeae or Moraceae families and this group includes in particular oil linen, fiber linen (flax), nettles such as nettles, ramie, hemp or hops. Flax is particularly preferred.
  • the vegetable substrate is digested in an aqueous solution which preferably contains 2.5 to 20 g of trisodium phosphate per liter of water and preferably 3 to 10 g, in particular 3.5 to 8.5 g, but more preferably 5 to Contains 7 g of trisodium phosphate per liter of water.
  • this digestion solution preferably also contains a dispersing agent and / or a bleaching agent. If the bleaching agent is present in the digestion solution at the same time, a shortening of the process is even advantageously possible since subsequent bleaching of the cellulose fiber material obtained, if desired, can be omitted. The cost savings for this can be considerable.
  • any agent suitable for this purpose in such digestion solutions can be used as the dispersing agent, but preferably water glass or a surfactant or a surfactant mixture is used, suitable surfactants and surfactant mixtures preferably containing anionic surfactant and possibly small additions of nonionic components.
  • a suitable surfactant product is, for example, Cottoclarin® from Henkel.
  • the bleaching agent is preferably hydrogen peroxide, which can be used, for example, in the form of a 35% aqueous solution.
  • hydrogen peroxide preferably hydrogen peroxide
  • other known bleaching agents suitable for cellulose fiber bleaching can also be used.
  • the amount of dispersant present in the digestion solution is preferably in the range from 0.5 to 10 g / 1, in particular 1 to 5 g / 1 and preferably 3 g / 1.
  • the bleaching agent is present in the digestion solution in an amount of preferably 0.1 to 15 g / 1, in particular 1 to 10 g / 1 and preferably 5 to 8 g / 1, in the case of hydrogen peroxide in the form a 35% aqueous solution according to a preferred embodiment, 8 ml of this hydrogen peroxide solution per liter of digestion solution can also be used.
  • the vegetable substrate is simultaneously with the digestion by the trisodium phosphate with borax treated or pretreated with an aqueous borax solution before digestion by the trisodium phosphate.
  • the amount of borax present in this simultaneous treatment or in this pretreatment solution is preferably in the range from 0.5 to 10 g / 1, in particular 1 to 5 g / 1 and preferably 3 g / 1.
  • the pretreatment of the vegetable substrate with this solution is preferably carried out at a temperature of 30 to 60 ° C., preferably 40 to 50 ° C. and in particular at 45 ° C. This pretreatment advantageously enables a higher degree of bleaching of the cellulose fiber material obtained, the bleaching preferably taking place simultaneously with the digestion.
  • the vegetable substrate can also be disrupted in two successive identical sub-stages. Between these stages, the part of the undesired accompanying cellulose fiber substances dissolved up to that point can be removed. This two-step procedure facilitates the extensive or complete removal of these substances.
  • the cooking solution used for this purpose is drained off and the residue is rinsed with water, which preferably has a temperature which corresponds to the drained solution or can be somewhat lower.
  • the container with the washed residue is then refilled with water, it being possible for the water to be adjusted to a pH of about 8, for example with trisodium phosphate.
  • the water used for rinsing can also be treated accordingly.
  • the cellulose fiber material obtained is then treated with an enzyme or enzyme mixture in the aqueous solution adjusted to a pH of 8.
  • an enzyme or enzyme mixture in the aqueous solution adjusted to a pH of 8.
  • pectases and lignases can also be present in an enzyme mixture.
  • a suitable enzyme product for starch degradation is, for example, Thermamyl from Novo Nordisk.
  • the enzyme or enzyme mixture or enzyme product can be used in an amount of 1 to 10 ml per liter of water, in particular 2 to 8 and preferably 3 to 5 ml per liter of water.
  • After the enzyme treatment is rinsed again and the cellulose fiber material obtained is dried.
  • the pH of the water can be changed as needed depending on the enzyme used. With Thermamyl ® as enzyme, a pH of 8 is preferred.
  • Another advantage of the method according to the invention is that the pectins and calcium pectinates removed after or during the digestion can be recovered in a form in which the gelling ability has largely been retained.
  • the mixture was made up with water which had a temperature of 70 ° C. and a pH of 8.0 (trisodium phosphate) and contained 3 ml / l of the enzyme Thermomyl.
  • the substrate to be treated was left in this bath for 30 minutes. It was then rinsed twice with water at a temperature of 45 ° C. and dried.
  • the cellulose fiber material obtained had the following properties:
  • the properties of the cellulose fiber material obtained corresponded to those of the product from Example 1.

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  • Paper (AREA)

Abstract

The invention concerns a method of obtaining cellulose fibre material from a plant substrate containing calcium pectinate, the plant substrate being solubilized by using trisodium phosphate and optionally bleached. The method is characterized in that the plant substrate is simultaneously treated with borax or pretreated with an aqueous borax solution before solubilization. Preferably the borax is present in an amount of between 0.5 and 10 g, in particular between 1 and 5 g and preferably 3 g per litre of water and the temperature of the solution is in particular between 30 and 60 °C, preferably between 40 and 50 °C and more preferably 45 °C.

Description

Verfahren zur Gewinnung von Cellulosefasermaterial aus Calciumpektinat-haltiσem, pflanzlichem Substrat Process for the production of cellulose fiber material from calcium pectinate-containing plant substrate
Die Erfindung betrifft ein Verfahren zur Gewinnung von Cellulo¬ sefasermaterial aus Calciumpektinat-haltigem, pflanzlichem Sub¬ strat .The invention relates to a process for the production of cellulose fiber material from vegetable substrate containing calcium pectinate.
Pflanzliche Substrate werden seit langer Zeit zur Herstellung von Cellulosefasermaterialien verwendet. Ein solches Material ist beispielsweise Zellstoff, der in der Regel aus Holz gewonnen wird und ein wichtiges Handelεprodukt ist, das für die Papier¬ herstellung verwendet wird. Zur Klasse der Cellulosefasern gehö¬ ren auch sogenanntes Sklerenchym- oder Bastfasern, die das Stützgewebe von Pflanzen wie Halme oder Stämme bilden. Diese Fasern liegen in der Natur immer in Kombination mit Substanzen wie Ligninen und Pektinen vor. Diese Begieitsubstanzen müssen entfernt werden, wenn das Cellulosefasermaterial in einer zur Weiterverarbeitung geeigneten Form gewonnen werden soll .Vegetable substrates have been used for a long time for the production of cellulose fiber materials. Such a material is, for example, cellulose, which is generally obtained from wood and is an important commercial product that is used for paper production. The class of cellulose fibers also includes so-called sclerenchyma or bast fibers, which form the supporting tissue of plants such as stalks or stems. In nature, these fibers are always in combination with substances such as lignins and pectins. These accompanying substances must be removed if the cellulose fiber material is to be obtained in a form suitable for further processing.
Bei den bekannten Verfahren zu Cellulosefasergewinnung wird das eingesetzte pflanzliche Substrat aufgeschlossen, entholzt, ent- pektiniert und je nach Wunsch gegebenenfalls auch gebleicht. Bei den zur Zeit wichtigsten und in technischem Maßstab zur Zell¬ stoffhersteliung eingesetzten Verfahren wird das Rohmaterial mittels Natronlauge aufgeschlossen. Hierbei können unterschied¬ liche Zusatzchemikalien vorhanden sein. Beispielsweise gibt es den sogenannten Natronaufschluß (NaOH, Na2C03), das Sulfidver¬ fahren (CaO, MgO, NaOH, NH4OH/S02) und das Sulfatverfahren (NaOH, Na2S, Na2C03) . Die genannten Chemikalien bilden jeweils die soge¬ nannten "Kochsäuren". Der Aufschluß bewirkt in erster Linie die Entlignifizierung (Entholzung) des Pflanzensubstrats, wobei die in dem Substrat enthaltenen Lignine in eine lösliche Form über¬ führt werden.In the known methods for cellulose fiber production, the plant substrate used is digested, de-wooded, de-pectinized and, if necessary, also bleached. The raw material is the most important and currently used on a technical scale for cellulose production digested with sodium hydroxide solution. Different additional chemicals can be present here. For example, there is the so-called sodium digestion (NaOH, Na 2 CO 3 ), the sulfide process (CaO, MgO, NaOH, NH 4 OH / SO 2 ) and the sulfate process (NaOH, Na 2 S, Na 2 CO 3 ). The chemicals mentioned each form the so-called "cooking acids". The digestion primarily results in the delignification (de-lignification) of the plant substrate, the lignins contained in the substrate being converted into a soluble form.
Die bekannten Verfahren haben jedoch den Nachteil, daß neben der gewünschten Entlignifizierung auch die Cellulosefasern in erheb¬ lichem Ausmaß angegriffen werden. Hierdurch wird u.a. die Fe¬ stigkeit des am Ende gewonnenen Zellstoffs erniedrigt. Auch die Zellstoffausbeute sinkt. Es wird daher nicht nur das Lignin gelöst sondern auch ein Teil der interessierenden Cellulosefa- sern unerwünschterweise zerstört. Es wird angenommen, daß der Polymerisationsgrad verringert bzw. die Faserlänge verkürzt wird. Ein Teil der Cellulose geht sogar in Lösung.However, the known methods have the disadvantage that, in addition to the desired delignification, the cellulose fibers are also attacked to a considerable extent. This means that the strength of the pulp obtained at the end is reduced. The cellulose yield also drops. Therefore, not only is the lignin dissolved, but also some of the cellulose fibers of interest are undesirably destroyed. It is believed that the degree of polymerization is reduced or the fiber length is shortened. Some of the cellulose even goes into solution.
Die bekannten Aufschlußverfahren rufen ferner aufgrund der zu entsorgenden Abfallprodukte Probleme hervor, wobei insbesondere die Abwasserfrage ein wichtiger Aspekt ist.The known digestion processes also cause problems due to the waste products to be disposed of, the waste water question in particular being an important aspect.
Neben den Ligninen sind jedoch auch die in den Pflanzensubstra¬ ten vorhandenen Pektine und Calciumpektinate zu entfernen, wobei insbesondere die Calciumpektinate in der Regel Schwierigkeiten bereiten.In addition to the lignins, however, the pectins and calcium pectinates present in the plant substrates must also be removed, the calcium pectinates in particular generally causing difficulties.
Der Erfindung liegt daher die Aufgabe zugrunde, ein neues Ver¬ fahren zur Gewinnung von Cellulosefasermaterial aus Calciumpek¬ tinat-haltigem, pflanzlichem Substrat zur Verfügung zu stellen, bei dem die Cellulosefasern nicht geschädigt werden, im Ver¬ gleich zu den bekannten Verfahren die Umwelt weniger belastet und die Verfahrensdauer verkürzt werden kann. Diese Aufgabe wird durch ein Verfahren gelöst, bei dem das pflanzliche Substrat aufgeschlossen und gegebenenfalls gebleicht wird, wobei das Verfahren dadurch gekennzeichnet ist, daß zum Aufschließen Trinatriumphosphat verwendet.The invention is therefore based on the object of providing a new process for the production of cellulose fiber material from plant substrate containing calcium pectinate, in which the cellulose fibers are not damaged, compared to the known processes the environment less burdened and the duration of the procedure can be shortened. This object is achieved by a process in which the vegetable substrate is digested and optionally bleached, the process being characterized in that trisodium phosphate is used for the digesting.
Bevorzugte Ausführungsformen des erfindungsgemäßen Verfahrens sind Gegenstand der Unteransprüche.Preferred embodiments of the method according to the invention are the subject of the dependent claims.
Erfindungsgemäß wird anstelle der in den bisher bekannten Auf- schlußverfahren verwendeten und die Cellulosefasern angreifenden Chemikalien (NaOH, Na-,C03; CaO, MgO, NaOH, NH4OH/S02; oder NaOH, Na2S, Na2C03) nunmehr Trinatriumphosphat eingesetzt.According to the invention, instead of the chemicals used in the digestion processes known hitherto and attacking the cellulose fibers (NaOH, Na-, C0 3 ; CaO, MgO, NaOH, NH 4 OH / S0 2 ; or NaOH, Na 2 S, Na 2 C0 3 ) now used trisodium phosphate.
Dies hat den Vorteil, daß einerseits die Lignine und Pektine, insbesondere Calciumpektinate, in ausreichendem Ausmaß und vor¬ zugsweise vollständig entfernt werden, andererseits aber die Cellulosefasern im wesentlichen geschont werden, wodurch die Produktqualität ausgesprochen gut ist und die Weiterverarbeitung und Entsorgungsprobleme vereinfacht bzw. vermindert werden.This has the advantage that on the one hand the lignins and pectins, in particular calcium pectinates, are removed to a sufficient extent and preferably completely, but on the other hand the cellulose fibers are essentially spared, whereby the product quality is extremely good and the further processing and disposal problems are simplified or reduced become.
Trinatriumphosphat wird üblicherweise zum Enthärten von Wasser wie Kesselspeisewasser , zum Phosphatieren , als Bestandteil von Seif enpulvern und Toilettenseifen , in Geschirrspülmitteln oder als Puf fer verwendet .Trisodium phosphate is usually used for softening water such as boiler feed water, for phosphating, as a component of soap powders and toilet soaps, in dishwashing detergents or as a buffer.
Das in dem beanspruchten Verfahren verwendete pflanzliche Sub¬ strat ist vorzugsweise aus Pflanzen der Familien Linaceae, Urti- caeae oder Moraceae ausgewählt und diese Gruppe umfaßt insbeson¬ dere Ölleinen, Faserleinen (Flachs), Nesseln wie Brennesseln, Ramie, Hanf oder Hopfen. Besonders bevorzugt ist Flachs.The vegetable substrate used in the claimed process is preferably selected from plants of the Linaceae, Urticaeae or Moraceae families and this group includes in particular oil linen, fiber linen (flax), nettles such as nettles, ramie, hemp or hops. Flax is particularly preferred.
Bei dem erfindungsgemäßen Verfahren wird das pflanzliche Sub¬ strat in einer wäßrigen Lösung aufgeschlossen, die vorzugsweise 2,5 bis 20 g Trinatriumphosphat pro Liter Wasser enthält und vorzugsweise 3 bis 10 g, insbesondere 3,5 bis 8,5 g, bevorzugter jedoch 5 bis 7 g Trinatriumphosphat pro Liter Wasser enthält. Diese Aufschlußlösung enthält neben dem AufSchlußmittel Trina¬ triumphosphat vorzugsweise auch ein Dispergiermittel und/oder ein Bleichmittel. Bei gleichzeitiger Anwesenheit des Bleichmit¬ tels in der Aufschlußlösung ist sogar vorteilhafterweise eine Verfahrensverkürzung möglich, da eine spätere, gegebenenfalls gewünschte Bleichung des erhaltenen Cellulosefasermaterials entfallen kann. Die Kostenersparnis hierfür kann beträchtlich sein.In the process according to the invention, the vegetable substrate is digested in an aqueous solution which preferably contains 2.5 to 20 g of trisodium phosphate per liter of water and preferably 3 to 10 g, in particular 3.5 to 8.5 g, but more preferably 5 to Contains 7 g of trisodium phosphate per liter of water. In addition to the disintegrant trinium phosphate, this digestion solution preferably also contains a dispersing agent and / or a bleaching agent. If the bleaching agent is present in the digestion solution at the same time, a shortening of the process is even advantageously possible since subsequent bleaching of the cellulose fiber material obtained, if desired, can be omitted. The cost savings for this can be considerable.
Als Dispergiermittel ist jedes für diese Zwecke in solchen Auf¬ schlußlösungen geeignete Mittel verwendbar, vorzugsweise wird aber Wasserglas oder ein Tensid bzw. ein Tensidgemisch verwen¬ det, wobei geeignete Tenside und Tensidgemische vorzugsweise anionisches Tensid und gegebenfalls geringe Zusätze an nichtio- nischen Komponenten enthalten. Ein geeignetes Tensidprodukt ist beispielsweise Cottoclarin ® der Firma Henkel.Any agent suitable for this purpose in such digestion solutions can be used as the dispersing agent, but preferably water glass or a surfactant or a surfactant mixture is used, suitable surfactants and surfactant mixtures preferably containing anionic surfactant and possibly small additions of nonionic components. A suitable surfactant product is, for example, Cottoclarin® from Henkel.
Bei dem Bleichmittel handelt es sich vorzugsweise um Wasser¬ stoffperoxid, das beispielsweise in Form einer 35 %-igen wäß- rigen Lösung eingesetzt werden kann. Es sind jedoch auch andere bekannte und zur Cellulosefaserbleichung geeignete Bleichmittel verwendbar.The bleaching agent is preferably hydrogen peroxide, which can be used, for example, in the form of a 35% aqueous solution. However, other known bleaching agents suitable for cellulose fiber bleaching can also be used.
Die in der Aufschlußlösung vorhandene Menge an Dispergiermittel liegt vorzugsweise im Bereich von 0,5 bis 10 g/1, insbesondere 1 bis 5 g/1 und bevorzugt 3 g/1. Das Bleichmittel ist in der Aufschlußlösung, falls vorhanden, in einer Menge von vorzugs¬ weise 0,1 biε 15 g/1, insbesondere 1 bis 10 g/1 und bevorzugt 5 bis 8 g/1 zugegen, wobei im Fall von Wasserstoffperoxid in Form einer 35 %-igen wäßrigen Lösung gemäß einer bevorzugten Ausfüh¬ rungsform auch 8 ml dieser Wasserstoffperoxidlösung pro Liter Aufschlußlösung verwendet werden können.The amount of dispersant present in the digestion solution is preferably in the range from 0.5 to 10 g / 1, in particular 1 to 5 g / 1 and preferably 3 g / 1. If available, the bleaching agent is present in the digestion solution in an amount of preferably 0.1 to 15 g / 1, in particular 1 to 10 g / 1 and preferably 5 to 8 g / 1, in the case of hydrogen peroxide in the form a 35% aqueous solution according to a preferred embodiment, 8 ml of this hydrogen peroxide solution per liter of digestion solution can also be used.
In einer weiteren bevorzugten Ausführungsform des erfindungs- gemäßen Verfahrens wird das pflanzliche Substrat gleichzeitig mit dem Aufschließen durch das Trinatriumphosphat mit Borax behandelt oder vor dem Aufschließen durch das Trinatriumphosphat mit einer wäßrigen Boraxlösung vorbehandelt. Die bei dieser gleichzeitigen Behandlung oder in dieser Vorbehandlungslösung vorhandene Menge Borax liegt vorzugsweise im Bereich von 0,5 bis 10 g/1, insbesondere 1 bis 5 g/1 und bevorzugt bei 3 g/1. Die Vorbehandlung des pflanzlichen Substrats mit dieser Lösung wird vorzugsweise bei einer Temperatur von 30 bis 60° C, bevorzugt 40 bis 50 °C und insbesondere bei 45° C durchgeführt. Diese Vorbehandlung ermöglicht vorteilhafterweise einen höheren Bleichgrad des gewonnenen Cellulosefasermaterials, wobei die Bleichung vorzugsweise gleichzeitig mit dem Aufschluß erfolgt.In a further preferred embodiment of the method according to the invention, the vegetable substrate is simultaneously with the digestion by the trisodium phosphate with borax treated or pretreated with an aqueous borax solution before digestion by the trisodium phosphate. The amount of borax present in this simultaneous treatment or in this pretreatment solution is preferably in the range from 0.5 to 10 g / 1, in particular 1 to 5 g / 1 and preferably 3 g / 1. The pretreatment of the vegetable substrate with this solution is preferably carried out at a temperature of 30 to 60 ° C., preferably 40 to 50 ° C. and in particular at 45 ° C. This pretreatment advantageously enables a higher degree of bleaching of the cellulose fiber material obtained, the bleaching preferably taking place simultaneously with the digestion.
Das Aufschließen des pflanzlichen Substrats kann auch in zwei aufeinanderfolgenden identischen Teilstufen vorgenommen werden. Zwischen diesen Stufen kann der bis dahin gelöste Teil der un¬ erwünschten Cellulosefaserbegleitsubstanzen entfernt werden. Dieses zweistufige Vorgehen erleichtert die weitgehende oder vollständige Entfernung dieser Substanzen.The vegetable substrate can also be disrupted in two successive identical sub-stages. Between these stages, the part of the undesired accompanying cellulose fiber substances dissolved up to that point can be removed. This two-step procedure facilitates the extensive or complete removal of these substances.
Nach dem Aufschließen des pflanzlichen Substrats wird die hierzu verwendete Kochlösung abgelassen und der Rückstand mit Wasser gespült, das vorzugsweise eine Temperatur aufweist, die der abgelassenen Lösung entspricht oder etwas niedriger sein kann. Anschließend wird der Behälter mit dem gewaschene Rückstand erneut mit Wasser aufgefüllt, wobei das Wasser beispielsweise mit Trinatriumphosphat auf einen pH-Wert von etwa 8 eingestellt sein kann. Auch das zum Spülen verwendete Wasser kann entspre¬ chend behandelt sein.After disintegrating the vegetable substrate, the cooking solution used for this purpose is drained off and the residue is rinsed with water, which preferably has a temperature which corresponds to the drained solution or can be somewhat lower. The container with the washed residue is then refilled with water, it being possible for the water to be adjusted to a pH of about 8, for example with trisodium phosphate. The water used for rinsing can also be treated accordingly.
Gemäß einer bevorzugten Ausführungsform wird das gewonnene Cel¬ lulosefasermaterial anschließend in der auf einen pH-Wert von 8 eingestellten wäßrigen Lösung mit einem Enzym oder Enzymgemisch behandelt. Hierdurch soll hauptsächlich die neben der Cellulose vorhandene Stärke abgebaut werden. Hierfür sind alle diesbezüg- lieh geeigneten Enzyme einsetzbar. Beispielsweise können in einem Enzymgemisch auch Pektasen und Lignasen vorhanden sein. Ein geeignetes Enzymprodukt für den Stärkeabbau ist beispiels- weise Thermamyl der Firma Novo Nordisk. Das Enzym oder Enzymge¬ misch bzw. Enzymprodukt kann in einer Menge von 1 bis 10 ml pro Liter Wasser, insbesondere 2 bis 8 und bevorzugt 3 bis 5 ml pro Liter Wasser verwendet. Nach der Enzymbehandlung wird erneut gespült und das gewonnene Cellulosefasermaterial getrocknet. Der pH-Wert des Wassers kann je nach Bedarf in Abhängigkeit von dem verwendeten Enzym verändert werden. Bei Thermamyl ® als Enzym ist ein pH-Wert von 8 bevorzugt.According to a preferred embodiment, the cellulose fiber material obtained is then treated with an enzyme or enzyme mixture in the aqueous solution adjusted to a pH of 8. This is mainly intended to break down the starch present in addition to cellulose. All suitable enzymes can be used for this. For example, pectases and lignases can also be present in an enzyme mixture. A suitable enzyme product for starch degradation is, for example, Thermamyl from Novo Nordisk. The enzyme or enzyme mixture or enzyme product can be used in an amount of 1 to 10 ml per liter of water, in particular 2 to 8 and preferably 3 to 5 ml per liter of water. After the enzyme treatment is rinsed again and the cellulose fiber material obtained is dried. The pH of the water can be changed as needed depending on the enzyme used. With Thermamyl ® as enzyme, a pH of 8 is preferred.
In samtlich verwendeten Behandlungslösungen können auch sonstige übliche Zusatzstoffe vorhanden sein, wobei diese jedoch die gewünschten Wirkungen der Hauptkomponente dieser Losungen nicht beeinträchtigen sollten und gegebenenfalls deshalb wegzulassen sind.Other customary additives may also be present in all treatment solutions used, although these should not impair the desired effects of the main component of these solutions and may therefore have to be omitted.
Ein weiterer Vorteil des erfindungsgemäßen Verfahrens besteht darin, daß die nach oder während des Aufschließens entfernten Pektine und Calciumpektinate in einer Form zurückgewonnen werden können, in der die Gelierfähigkeit weitgehend erhalten geblieben ist.Another advantage of the method according to the invention is that the pectins and calcium pectinates removed after or during the digestion can be recovered in a form in which the gelling ability has largely been retained.
Das erfindungsgemäße Verfahren wird nun anhand eines Beispiels einer bevorzugten Ausführungsform beschrieben.The method according to the invention will now be described using an example of a preferred embodiment.
Beispiel 1example 1
Es wurden 900 g zu behandelndes pflanzliches Substrat, Flachs in Form von sogenanntem Flachswerg, eingesetzt. Zunächst wurde das Substrat zum Einweichen und zur Vorbehandlung in 9 1 einer Lo¬ sung gegeben, die 3 g/1 Lösung an Borax enthielt. Diese Lösung wurde von 25° C mit einer Rate von 1,5° C/min auf 45° C erwärmt und anschließend 20 Minuten lang bei dieser Temperatur gehalten. Die Lösung wurde abgelassen und eine wäßrige Lösung zugeführt, die 5 g/1 Trinatriumphosphat, 3 g/1 Wasserglas und 8 ml/1 Was¬ serstoffperoxidlösung (35 %) enthielt. Diese Lösung hatte eben- falls eine Temperatur von 45° C. Dann wurde mit einer Rate von 2° C/min auf 110° C erhitzt und anschließend 60 Minuten lang bei dieser Temperatur gehalten. Danach wurde die Lösung auf eine Temperatur von etwa 80° C abgekühlt und abgelassen. Es wurde zweimal mit Wasser auf das vorherige Volumen aufgefüllt, wobei das Wasser eine Temperatur von 70° C besaß und jeder Spülvorgang (in dem aufgefüllten Bad) 10 Minuten dauerte.900 g of vegetable substrate to be treated, flax in the form of so-called flax tow, were used. The substrate was first placed in 9 l of a solution containing 3 g / l of borax solution for soaking and pretreatment. This solution was heated from 25 ° C at a rate of 1.5 ° C / min to 45 ° C and then held at that temperature for 20 minutes. The solution was drained and an aqueous solution was fed which contained 5 g / 1 trisodium phosphate, 3 g / 1 water glass and 8 ml / 1 hydrogen peroxide solution (35%). This solution had if a temperature of 45 ° C. It was then heated to 110 ° C at a rate of 2 ° C / min and then held at this temperature for 60 minutes. The solution was then cooled to a temperature of approximately 80 ° C. and discharged. It was filled twice with water to the previous volume, the water being at a temperature of 70 ° C. and each rinsing process (in the filled bath) taking 10 minutes.
Nach dem Spülvorgang wurde mit Wasser aufgefüllt, das eine Tem- peratur von 70° C und einem pH-Wert von 8,0 (Trinatriumphosphat) aufwies und 3 ml/1 des Enzyms Thermomyl enthielt. Das zu behan¬ delnde Substrat wurde 30 Minuten lang in diesem Bad belassen. Anschließend wurde zweimal mit Wasser mit einer Temperatur von 45° C gespült und getrocknet.After the rinsing process, the mixture was made up with water which had a temperature of 70 ° C. and a pH of 8.0 (trisodium phosphate) and contained 3 ml / l of the enzyme Thermomyl. The substrate to be treated was left in this bath for 30 minutes. It was then rinsed twice with water at a temperature of 45 ° C. and dried.
Das erhaltene Cellulosefasermaterial wies die folgenden Eigen¬ schaften auf:The cellulose fiber material obtained had the following properties:
Weißgrad 70 (ISO) gute SpinnbarkeitWhiteness 70 (ISO) good spinnability
Beispiel 2Example 2
Anstelle von 5 g/1 Trinatriumphosphat und 3 g/1 Wasserglas in der Aufschlußlösung wurden 7 g/1 Trinatriumphosphat und 3 g/1 Cottoclarin verwendet. Dies hat Vorteile bei der Filtrierung der Abwasserlauge.Instead of 5 g / 1 trisodium phosphate and 3 g / 1 water glass in the digestion solution, 7 g / 1 trisodium phosphate and 3 g / 1 cottoclarin were used. This has advantages when filtering the waste water liquor.
Die Eigenschaften des erhaltenen Cellulosefasermaterials ent¬ sprachen denjenigen des Produkts von Beispiel 1. The properties of the cellulose fiber material obtained corresponded to those of the product from Example 1.

Claims

Patentansprüche claims
1. Verfahren zur Gewinnung von Cellulosefasermaterial aus Cal- ciumpektinat-haltigem, pflanzlichem Substrat, bei dem das pflanzliche Substrat unter Verwendung von Trinatriumphσsphat aufgeschlossen und gegebenenfalls gebleicht wird, dadurch gekennzeichnet, daß das pflanzliche Substrat gleichzeitig mit Borax behandelt wird oder vor dem Aufschließen mit einer wäßrigen Boraxlösung vorbehandelt wird, wobei vorzugsweise Borax in einer Menge von 0,5 bis 10 g, insbesondere 1 bis 5 g und bevorzugt 3 g pro Liter Wasser vorhanden ist und die Temperatur der Lösung insbesondere 30 bis 60 °C, vorzugs¬ weise 40 bis 50 °C und bevorzugter 45 °C beträgt.1. A process for the production of cellulose fiber material from calcium pectinate-containing, vegetable substrate, in which the vegetable substrate is digested using trisodium phosphate and optionally bleached, characterized in that the vegetable substrate is treated simultaneously with borax or before digesting with a aqueous borax solution is pretreated, preferably borax in an amount of 0.5 to 10 g, in particular 1 to 5 g and preferably 3 g per liter of water and the temperature of the solution in particular 30 to 60 ° C., preferably 40 to 50 ° C and more preferably 45 ° C.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das pflanzliche Substrat ausgewählt ist aus Pflanzen der Familien Linaceae, Urticaeae oder Moraceae und insbesondere aus Ölleinen, Faserleinen (Flachs), Nesseln wie Brennesseln, Ramie, Hanf oder Hopfen.2. The method according to claim 1, characterized in that the vegetable substrate is selected from plants of the families Linaceae, Urticaeae or Moraceae and in particular from oil linen, fiber linen (flax), nettles such as nettles, ramie, hemp or hops.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das pflanzliche Substrat in einer Lösung aufgeschlossen wird, die 2,5 bis 20 g, vorzugsweise 3 bis 10 g, insbesonde¬ re 3,5 bis 8,5 g und bevorzugt 5 bis 7 g Trinatriumphosphat pro Liter Wasser enthält.3. The method according to claim 1 or 2, characterized in that the vegetable substrate is digested in a solution which 2.5 to 20 g, preferably 3 to 10 g, in particular 3.5 to 8.5 g and preferably 5 contains up to 7 g of trisodium phosphate per liter of water.
4. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die Aufschlußlösung außerdem Dispergier¬ mittel und/oder Bleichmittel enthält, wobei das Dispergier¬ mittel vorzugsweise Wasserglas oder ein Tensid bzw. ein Tensidgemisch ist und das Bleichmittel vorzugsweise Wasser¬ stoffperoxid ist. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß das Dispergiermittel in einer Menge von 0,5 bis 10 g, insbesondere 1 bis 5 g und bevorzugt 3 g pro Liter Aufschlußlösung vorhanden ist und das Bleichmittel in einer Menge von 0,1 bis 15 g, insbesondere 1 bis 10 g und bevorzugt 5 bis 8 g pro Liter Aufschlußlösung vorhanden ist.4. The method according to any one of the preceding claims, characterized in that the digestion solution also contains dispersing agents and / or bleaching agents, the dispersing agent preferably being water glass or a surfactant or a surfactant mixture and the bleaching agent preferably being hydrogen peroxide. Method according to one of the preceding claims, characterized in that the dispersant is present in an amount of 0.5 to 10 g, in particular 1 to 5 g and preferably 3 g per liter of digestion solution and the bleaching agent in an amount of 0.1 to 15 g, in particular 1 to 10 g and preferably 5 to 8 g, per liter of digestion solution.
Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß das Bleichmittel eine Wasserstoffperoxidlösung (35%) ist und in einer Menge von 8 ml/1 vorhanden ist. A method according to claim 5, characterized in that the bleaching agent is a hydrogen peroxide solution (35%) and is present in an amount of 8 ml / 1.
EP95940192A 1995-11-17 1995-11-17 Method of obtaining cellulose fibre material from a plant substrate containing calcium pectinate Expired - Lifetime EP0861347B1 (en)

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EP0861347B1 EP0861347B1 (en) 2000-03-01

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DE102017011741A1 (en) 2017-12-19 2019-06-19 Hanffaser Uckermark eG Process for an enzymatic-surfactant fiber pulping of bast strips

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DK172928B1 (en) * 1998-05-01 1999-10-04 Landbrugets Radgvningcenter Process for making single fiber mats, fiber mats and using such a fiber mat.
DE102007030576A1 (en) 2007-07-02 2009-01-08 Flasin Faser Gmbh High-strength fiber material made of natural fiber, process for its production and its use for the production of composite materials
DE102009043428A1 (en) 2009-09-29 2011-04-07 Flasin Faser Gmbh Thin nonwoven fabric based on natural fibers and process for its production
DE102022003958A1 (en) 2022-10-24 2024-04-25 Hochschule Zittau/Görlitz Körperschaft des öffentlichen Rechts Method for parameter-controlled microbial digestion of bast fibres

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US2073682A (en) * 1935-06-13 1937-03-16 Jr Franklin R Chesley Processes of treating vegetable fibrous material for the production of cellulose fibe
CA1082859A (en) * 1976-07-05 1980-08-05 Larry D. Markham Pulping process using oxygen and sodium tetraborate
RU1808890C (en) * 1991-04-30 1993-04-15 Костромской технологический институт Method for production of flax stock
DE4420221C2 (en) * 1994-06-06 1996-10-31 Windi Winderlich Gmbh Process for the production of cellulose fiber material from vegetable substrate containing calcium pectinate

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Publication number Priority date Publication date Assignee Title
DE102017011741A1 (en) 2017-12-19 2019-06-19 Hanffaser Uckermark eG Process for an enzymatic-surfactant fiber pulping of bast strips

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DE59507926D1 (en) 2000-04-06
WO1997019221A1 (en) 1997-05-29
CZ146898A3 (en) 1998-09-16
EP0861347B1 (en) 2000-03-01

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