EP3212846A1 - Fast-fibrillating lyocell fibers, and use thereof - Google Patents

Fast-fibrillating lyocell fibers, and use thereof

Info

Publication number
EP3212846A1
EP3212846A1 EP15744462.1A EP15744462A EP3212846A1 EP 3212846 A1 EP3212846 A1 EP 3212846A1 EP 15744462 A EP15744462 A EP 15744462A EP 3212846 A1 EP3212846 A1 EP 3212846A1
Authority
EP
European Patent Office
Prior art keywords
fibers
lyocell fibers
pulp
lyocell
fibrillated
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
EP15744462.1A
Other languages
German (de)
French (fr)
Other versions
EP3212846B1 (en
Inventor
Johann Männer
Rudolf Aigner
Jim GANNON
Matt Riley
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.)
Lenzing AG
Original Assignee
Lenzing AG
Chemiefaser Lenzing AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lenzing AG, Chemiefaser Lenzing AG filed Critical Lenzing AG
Priority to PL15744462T priority Critical patent/PL3212846T3/en
Publication of EP3212846A1 publication Critical patent/EP3212846A1/en
Application granted granted Critical
Publication of EP3212846B1 publication Critical patent/EP3212846B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/02—Synthetic cellulose fibres
    • D21H13/08—Synthetic cellulose fibres from regenerated cellulose
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D04H1/492—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres by fluid jet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B1/00—Cleaning by methods involving the use of tools
    • B08B1/10—Cleaning by methods involving the use of tools characterised by the type of cleaning tool
    • B08B1/14—Wipes; Absorbent members, e.g. swabs or sponges
    • B08B1/143—Wipes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
    • D01D5/423—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by fibrillation of films or filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/425—Cellulose series
    • D04H1/4258—Regenerated cellulose series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43835—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43838—Ultrafine fibres, e.g. microfibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35—Abrasion, pilling or fibrillation resistance

Definitions

  • the present invention relates to fibrillated lyocell fibers containing a
  • Fibrillation quotient Q of 20 or greater and their content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 prn is at least 50%, as well as their use for producing a wipe, the pulp and 5 to 20 wt .-% fibrillated Contains lyocell fibers.
  • US 6042769 discloses a method of increasing the fibrillation tendency of lyocell fibers by a treatment which reduces the degree of polymerization of the cellulose by at least 200 units.
  • the fiber thus obtained should be used mainly in nonwovens and paper.
  • the treatment is preferably carried out with a bleaching agent, in particular with sodium hypochlorite.
  • the treatment with an acid, preferably a mineral acid such as hydrochloric acid, sulfuric acid or
  • regenerated cellulose fibers such as viscose and lyocell in nonwovens
  • lyocell fibers are fibrillated and used as cellulose microfibers in admixture with paper pulp in so-called wet-laying processes (also referred to in the art as "wet-laid processes").
  • wet-laying processes also referred to in the art as "wet-laid processes”
  • wipes and paper structures for example. Tissues made.
  • US 8187422 describes that by incorporating fibrillated lyocell microfibers into paper pulp, the properties of disposable cellulosic wipes can be optimized accordingly.
  • the cleaning behavior should be correspondingly improved by this admixture.
  • the optimized property profile should be improved by an increased opacity (light scattering) and porosity, distinguished by the improvement of the soft grip. The higher porosity is said to result in a higher absorbency of water and oil, resulting in improved cleaning performance.
  • US 8187422 does not describe exactly how the lyocell microfibers used are made. It only indicates that conventional lyocell staple fibers, such as e.g. also be used for the production of textiles can be fibrillated in a disc refiner or similar aggregate in an aqueous medium at low solids content.
  • the Lyocell microfibers used according to US 8187422 were purchased in an already fibrillated state from a supplier. They have a fibrillation degree of CSF ⁇ 175 ml and a diameter of ⁇ 2 ⁇ . 40% of the fibers should have a fineness of finer than 14mesh.
  • the disposable wipes disclosed in US 8187422 contain between 25 and 75% of the thus prepared lyocell microfibers.
  • the object of this prior art was to provide fibers for use in wipes available, which can be fibrilliert for a cost-effective and on the other hand in a smaller proportion in wipes still the same mechanical
  • Lyocell fibers characterized in that they have a Fibrillation quotient Q of 20 or greater and their content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 pm is at least 50%.
  • Lyocell fibers in the context of the present invention does not mean a total amount of completely identical fibers, but a mixture of fibers of basically the same nature, wherein in the mixture fibers
  • tcsF2oo is the time (in minutes) required in the CSF check to reach a CSF value of 200.
  • a Q value of up to 400 can be achieved.
  • Another object of the present invention is a wipe containing pulp and 5 to 20% by weight of fibrillated lyocell fibers and wherein the fibrillated lyocell fibers have a fibrillation quotient Q of 20 or greater.
  • the pulp is a
  • the fast-fibrillating lyocell fibers could be prepared by acid treatment of conventional lyocell fibers.
  • This acid treatment can be carried out according to the invention by using a fiber cable extruded in a known manner by Lyocell method with a Einzelmaschinetiter of for example between 1, 0 and 6.0 dtex with dilute mineral acid, for example hydrochloric, sulfuric or nitric acid, with a concentration for example, between 0.5 and 5% at room temperature in a container at a liquor ratio of for example, impregnated 1:10 and then pressed to a certain residual moisture of, for example, 200%.
  • the impregnated fiber cable is then treated with water vapor at overpressure in a suitable
  • the fiber cable is cut to produce the wipes according to the invention in staple fibers suitable cut length, for example 4 to 6 mm.
  • the fibrillation can then take place in a comminution unit customary in the paper industry, for example a grinding unit, a refiner, a disintegrator or a hydrapulper. It is carried out there until the desired degree of fibrillation is reached.
  • the effect of acid treatment and consequent reduction of CSF can be influenced by varying the treatment parameters. With longer treatment duration in the overpressure steam can with smaller
  • Steam treatment can be influenced by the CSF value.
  • fast-fibrillating lyocell fibers according to the invention can be used according to the invention for the production of a wide variety of products, such as
  • Wiping cloths especially disposable wipes, papers, in particular filter papers and papers for technical applications such as batteries, etc. are used.
  • These and other products as well as the manufacturing processes in question are described inter alia in WO 95/35399, to which reference is hereby made and the disclosure thereof
  • wipes according to the invention can be prepared by basically known processes from the fibers and pulp according to the invention.
  • the fibers and pulp according to the invention can be prepared by basically known processes from the fibers and pulp according to the invention.
  • the present invention also relates to the use of the inventive fibers described above for producing a wipe, wherein the wipe comprises pulp and 5 to 20 wt .-% fibrillated lyocell fibers.
  • the pulp is preferably a paper pulp.
  • Fast fibrillating lyocell fibers are produced as follows: A lyocell fiber strand having a single fiber titer of 1.7 dtex is diluted with dilute sulfuric acid at room temperature and a
  • the impregnated fiber strand is subjected to steam in a laboratory damper for about 10 minutes under pressure, then washed free of acid with water and dried.
  • the dry fiber strand becomes 5mm
  • the fibrillation tendency is measured by means of a CSF (Canadian Standard of Freeness) test according to TAPPI Standard T227 om-94 and the fibrillation quotient Q is determined. Compared:
  • Fig. 1 shows the decrease of the CSF value with increasing
  • Lyocell fibers significantly less time and energy than when using untreated Lyocell fibers.
  • Table 1 shows the tcsF2oo values determined for the various samples and the Q values calculated from them.
  • Example 1 The same fiber samples were compared as in Example 1:
  • Each 1% aqueous fiber suspensions of both fiber samples A and B were ground in a laboratory refiner Andritz R1 L at a power of 500W, both the energy consumption in kWh / to and the duration to achieve a degree of grinding of CSF 200 (Canadian Standard of Freeness test according to TAPPI Standard T227 om-94).
  • the fibrillating lyocell fiber could be processed in less than 80% of the energy consumption compared to the standard lyocell fiber in only 50% of the milling time (see Table 2).
  • FIG. 2 shows an SEM image of the leaf from the suspension of sample B.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Paper (AREA)
  • Cleaning Implements For Floors, Carpets, Furniture, Walls, And The Like (AREA)
  • Artificial Filaments (AREA)

Abstract

The present invention relates to fibrillated lyocell fibers which have a fibrillation ratio Q of 20 or more and whose content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 μm is at least 50%, and to the use of said fibers for producing a wipe which contains cellulosic fibers and 5 to 20 wt.% lyocell fibers.

Description

Schnell fibrillierende Lyocellfasern und deren Verwendung  Fast fibrillating lyocell fibers and their use
Die vorliegende Erfindung betrifft fibrillierte Lyocellfasern, die einen The present invention relates to fibrillated lyocell fibers containing a
Fibrillationsquotienten Q von 20 oder größer aufweisen und deren Gehalt an Mikrofasern mit einer Feinheit von kleiner 14 mesh und einem Durchmesser von kleiner 2 prn mindestens 50% beträgt, sowie deren Verwendung zur Herstellung eines Wischtuches, das Zellstoff und 5 bis 20 Gew.-% fibrillierte Lyocellfasern enthält. Fibrillation quotient Q of 20 or greater and their content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 prn is at least 50%, as well as their use for producing a wipe, the pulp and 5 to 20 wt .-% fibrillated Contains lyocell fibers.
Stand der Technik State of the art
Die US 6042769 offenbart ein Verfahren, mit dem die Fibrillationsneigung von Lyocell-Fasern durch eine Behandlung, die den Polymerisationsgrad der Cellulose um mindestens 200 Einheiten herabsetzt, erhöht wird. Die so erhaltene Faser sollte vor allem in Vliesstoffen und Papier eingesetzt werden. Bevorzugt erfolgt die Behandlung mit einem Bleichmittel, insbesondere mit Natriumhypochlorit. Alternativ ist auch die Behandlung mit einer Säure, vorzugsweise einer Mineralsäure wie Salzsäure, Schwefelsäure oder US 6042769 discloses a method of increasing the fibrillation tendency of lyocell fibers by a treatment which reduces the degree of polymerization of the cellulose by at least 200 units. The fiber thus obtained should be used mainly in nonwovens and paper. The treatment is preferably carried out with a bleaching agent, in particular with sodium hypochlorite. Alternatively, the treatment with an acid, preferably a mineral acid such as hydrochloric acid, sulfuric acid or
Salpetersäure möglich. Dieses Verfahren wurde allerdings bis heute nicht kommerziell umgesetzt. Nitric acid possible. However, this process has not been implemented commercially until today.
Die Verwendung von Cellulose-Regeneratfasern, wie Viskose und Lyocell in Vliesstoffen ist hinlänglich bekannt. Im speziellen werden durch Mahlung oder auch in sogenannten Refinern, die aus der Papierherstellung bekannt sind, Lyocellfasern auffibrilliert und als Cellulose-Mikrofasern in Mischung mit Papierzellstoff in sogenannten Nasslege-Verfahren (in Fachkreisen auch als „wet-laid-Verfahren bezeichnet) eingesetzt. Dabei werden verschiedenste Produkte wie zB. Wisch- bzw. Reinigungstücher, sogenannte wipes, und Papierstrukturen für zB. Tissues, hergestellt. Beispielsweise beschreibt die US 8187422, daß durch die Beimischung fibrillierter Lyocell-Mikrofasern zu Papierzellstoff, die Eigenschaften von cellulosischen Einweg-Wischtüchern entsprechend optimiert werden können. Im Gegensatz zu reinen Zellstoff- Wischtüchern soll durch diese Beimischung das Reinigungsverhalten entsprechend verbessert werden. Dabei soll sich das optimierte Eigenschaftsprofil durch eine erhöhte Opazität (light scattering) und Porosität, bei Verbesserung des Weichgriffs auszeichnen. Die höhere Porosität soll ein höheres Saugvermögen für Wasser und Öl bedingen, was zu einem verbesserten Reinigungsverhalten führt. The use of regenerated cellulose fibers such as viscose and lyocell in nonwovens is well known. In particular, by grinding or in so-called refiners, which are known from papermaking, lyocell fibers are fibrillated and used as cellulose microfibers in admixture with paper pulp in so-called wet-laying processes (also referred to in the art as "wet-laid processes"). Here are a variety of products such as. Wiping or cleaning cloths, so-called wipes, and paper structures for example. Tissues made. For example, US 8187422 describes that by incorporating fibrillated lyocell microfibers into paper pulp, the properties of disposable cellulosic wipes can be optimized accordingly. In contrast to pure cellulose wipes, the cleaning behavior should be correspondingly improved by this admixture. The optimized property profile should be improved by an increased opacity (light scattering) and porosity, distinguished by the improvement of the soft grip. The higher porosity is said to result in a higher absorbency of water and oil, resulting in improved cleaning performance.
Die US 8187422 beschreibt nicht genau, wie die verwendeten Lyocell- Mikrofasern hergestellt werden. Sie deutet nur an, daß übliche Lyocell- Stapelfasern, wie sie z.B. auch für die Herstellung von Textilien eingesetzt werden, in einem Scheibenrefiner oder ähnlichem Aggregat in einem wässrigen Medium bei niedrigem Feststoffanteil fibrilliert werden können. Die gemäß der US 8187422 verwendeten Lyocell-Mikrofasern wurden in bereits fibrilliertem Zustand von einem Lieferant gekauft. Sie weisen einen Fibrillationsgrad von CSF < 175ml sowie einen Durchmesser von < 2μιη auf. 40% der Fasern sollen dabei eine Feinheit von feiner als 14mesh haben. Die in der US 8187422 offenbarten Einweg-Wischtücher enthalten zwischen 25 und 75% der auf diese Weise hergestellten Lyocell-Mikrofasern. US 8187422 does not describe exactly how the lyocell microfibers used are made. It only indicates that conventional lyocell staple fibers, such as e.g. also be used for the production of textiles can be fibrillated in a disc refiner or similar aggregate in an aqueous medium at low solids content. The Lyocell microfibers used according to US 8187422 were purchased in an already fibrillated state from a supplier. They have a fibrillation degree of CSF <175 ml and a diameter of <2μιη. 40% of the fibers should have a fineness of finer than 14mesh. The disposable wipes disclosed in US 8187422 contain between 25 and 75% of the thus prepared lyocell microfibers.
Die gemäß der US 8187422 eingesetzten Lyocellfasern fibrillieren zwar bei mechanischer Mahlbeanspruchung in einem wässrigen Medium. Allerdings ist der Aufwand, um gemäß der US 8187422 einen bestimmten Fibrillationsgrad zur erreichen, in Bezug auf Zeit und Energieeinsatz mit den derzeitigen Refiner-Technologien deutlich größer als beispielsweise für Zellstoff. Although the lyocell fibers used according to US Pat. No. 8,174,722 fibrillate on mechanical milling in an aqueous medium. However, the effort to achieve a certain level of fibrillation according to US 8187422 is significantly greater in time and energy use with current refining technologies than, for example, pulp.
Aufgabe task
Die Aufgabe bestand gegenüber diesem Stand der Technik darin, Fasern zur Verwendung in Wischtüchern zur Verfügung zu stellen, die zum einen kostengünstiger fibrilliert werden können und zum anderen in geringerem Mengenanteil in Wischtüchern noch die gleichen mechanischen The object of this prior art was to provide fibers for use in wipes available, which can be fibrilliert for a cost-effective and on the other hand in a smaller proportion in wipes still the same mechanical
Eigenschaften der Wischtücher, wie beispielsweise hohe Festigkeit, ermöglichen. Properties of the wipes, such as high strength allow.
Beschreibung der Erfindung Description of the invention
Die oben beschriebene Aufgabe konnte gelöst werden durch fibrillierte The above-described problem could be solved by fibrillated
Lyocellfasern, die dadurch gekennzeichnet sind, dass sie einen Fibrillationsquotienten Q von 20 oder größer aufweisen und ihr Gehalt an Mikrofasern mit einer Feinheit von kleiner 14 mesh und einem Durchmesser von kleiner 2 pm mindestens 50% beträgt. Um Missverständnisse zu vermeiden, soll hiermit klargestellt werden, daß der Begriff„fibrillierte Lyocell fibers, characterized in that they have a Fibrillation quotient Q of 20 or greater and their content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 pm is at least 50%. To avoid misunderstandings, it should be made clear that the term "fibrillated
Lyocellfasern" im Zusammenhang mit der vorliegenden Erfindung nicht eine Gesamtmenge völlig identischer Fasern bedeutet, sondern ein Gemisch von Fasern grundsätzlich gleicher Natur, wobei im Gemisch Fasern Lyocell fibers "in the context of the present invention does not mean a total amount of completely identical fibers, but a mixture of fibers of basically the same nature, wherein in the mixture fibers
unterschiedlicher Feinheit (gemessen in mesh) und unterschiedlichem different fineness (measured in mesh) and different
Durchmesser. Diameter.
Der Fibrillationsquotient Q ist definiert als Q = 200 / tCSF2oo The fibrillation quotient Q is defined as Q = 200 / t CS F2oo
Dabei ist tcsF2oo die Zeit (in min), die in der CSF-Prüfung benötigt werden, um einen CSF-Wert von 200 zu erreichen. Je größer Q ist, umso weniger Zeit wird also bei gleichbleibenden Fibrillierungsbedingungen benötigt, um den gleichen Fibrillationsgrad zu erreichen. Je nach Art der Ausgangsfasern und der erfindungsgemäßen Säurebehandlung kann ein Q-Wert von bis zu 400 erreicht werden. Where tcsF2oo is the time (in minutes) required in the CSF check to reach a CSF value of 200. The larger Q is, the less time is needed at constant fibrillation conditions to achieve the same degree of fibrillation. Depending on the nature of the starting fibers and the acid treatment according to the invention, a Q value of up to 400 can be achieved.
Ein weiterer Gegenstand der vorliegenden Erfindung ist ein Wischtuch, das Zellstoff und 5 bis 20 Gew.-% fibrillierte Lyocellfasern enthält und wobei die fibrillierten Lyocellfasern einen Fibrillationsquotienten Q von 20 oder größer aufweisen. In einer bevorzugten Ausführungsform ist der Zellstoff ein Another object of the present invention is a wipe containing pulp and 5 to 20% by weight of fibrillated lyocell fibers and wherein the fibrillated lyocell fibers have a fibrillation quotient Q of 20 or greater. In a preferred embodiment, the pulp is a
Papierzellstoff. Paper pulp.
Die schnell fibrillierenden Lyocell-Fasern konnten überraschenderweise durch eine Säurebehandlung von herkömmlichen Lyocellfasern hergestellt werden. Diese Säurebehandlung kann erfindungsgemäß erfolgen, indem ein auf bekannte Weise nach dem Lyocell-Verfahren aus Spinndüsen extrudiertes Faserkabel mit einem Einzelfasertiter von beispielsweise zwischen 1 ,0 und 6,0 dtex mit verdünnter Mineralsäure, beispielsweise Salz-, Schwefel- oder Salpetersäure, mit einer Konzentration von beispielsweise zwischen 0,5 und 5 % bei Raumtemperatur in einem Behälter bei einem Flottenverhältnis von beispielsweise 1 :10 imprägniert und dann auf eine gewisse Restfeuchte von beispielsweise 200% abgepresst wird. Das imprägnierte Faserkabel wird anschließend mit Wasserdampf bei Überdruck in einer geeigneten Surprisingly, the fast-fibrillating lyocell fibers could be prepared by acid treatment of conventional lyocell fibers. This acid treatment can be carried out according to the invention by using a fiber cable extruded in a known manner by Lyocell method with a Einzelfasertiter of for example between 1, 0 and 6.0 dtex with dilute mineral acid, for example hydrochloric, sulfuric or nitric acid, with a concentration for example, between 0.5 and 5% at room temperature in a container at a liquor ratio of for example, impregnated 1:10 and then pressed to a certain residual moisture of, for example, 200%. The impregnated fiber cable is then treated with water vapor at overpressure in a suitable
Vorrichtung beaufschlagt, danach säurefrei gewaschen und getrocknet. Applied device, then washed acid-free and dried.
Zur Ermittlung der Fibrillationsneigung wird das Faserkabel auf eine To determine the Fibrillationsneigung the fiber cable to a
Stapellänge von 5 mm geschnitten und der CSF-Prüfung (Canadian Standard Freeness gemäß TAPPI Standard T227 om-94) unterzogen. 5 mm cut and subjected to the CSF test (Canadian Standard Freeness according to TAPPI Standard T227 om-94).
Das Faserkabel wird zur Herstellung der erfindungsgemäßen Wischtücher in Stapelfasern geeigneter Schnittlänge, beispielsweise 4 bis 6 mm geschnitten. Die Fibrillierung kann dann in einem in der Papierindustrie gebräuchlichen Zerkleinerungsaggregat, beispielsweise einem Mahlaggregat, einem Refiner, einem Desintegrator oder einem Hydrapulper, stattfinden. Sie wird dort solange ausgeführt, bis der gewünschte Fibrillierungsgrad erreicht ist. The fiber cable is cut to produce the wipes according to the invention in staple fibers suitable cut length, for example 4 to 6 mm. The fibrillation can then take place in a comminution unit customary in the paper industry, for example a grinding unit, a refiner, a disintegrator or a hydrapulper. It is carried out there until the desired degree of fibrillation is reached.
Der Effekt der Säurebehandlung und der dadurch bedingten Reduzierung des CSF kann durch Variieren der Behandlungsparameter beeinflusst werden. Bei längerer Behandlungsdauer im Überdruck-Dampf kann mit geringeren The effect of acid treatment and consequent reduction of CSF can be influenced by varying the treatment parameters. With longer treatment duration in the overpressure steam can with smaller
Säurekonzentrationen der gleiche Effekt erzielt werden und umgekehrt. Acid concentrations of the same effect can be achieved and vice versa.
Ebenso kann mit niedrigeren oder höheren Temperaturen der Similarly, with lower or higher temperatures of the
Dampfbehandlung der CSF-Wert beeinflusst werden. Steam treatment can be influenced by the CSF value.
Dabei wird offenbar die Faserstruktur gezielt geschwächt und damit die Fibrillationsneigung erhöht. It seems that the fiber structure is deliberately weakened, thus increasing the fibrillation tendency.
Bei einer anschließenden CSF-Prüfung ist festzustellen, dass die Mahldauer, die benötigt wird, um einen CSF von 200ml zu erreichen, bei unbehandelten Lyocell-Fasern, je nach Zellstofftype und Produktionsparameter im Bereich von 12-16 Minuten beträgt (siehe Fig. 1). Dieses Vorgehen ist mit dem in US 8187422 vergleichbar. Die mit Säure behandelten Lyocell-Fasern benötigen bei gleicher Mahlungsart nur mehr ca. 3-4 Minuten bis zum Erreichen eines CSF von 200ml (Fig. 1). Zudem konnte festgestellt werden, dass sich durch die Säurevorbehandlung der Anteil an beim Mahlen gebildeten Mikrofasern mit <14 mesh und <2 pm Durchmesser deutlich auf über 50% erhöht. Dadurch ist es möglich, den Anteil an Lyocellfasern in einem Reinigungstuch auf deutlich < 25 Gew.-%, erfindungsgemäß sogar unter 20 Gew.% zu reduzieren und trotzdem die geforderten, beispielsweise in der US 8187422 beschriebenen Eigenschaftsprofile zu erhalten. In a subsequent CSF test, it should be noted that the milling time required to achieve a 200 ml CSF is in the range of 12-16 minutes for untreated Lyocell fibers, depending on pulp type and production parameters (see Fig. 1). , This procedure is comparable to that in US 8187422. The acid-treated lyocell fibers only require about 3-4 minutes for the same type of grinding to reach a CSF of 200 ml (FIG. 1). In addition, it was found that the proportion of microfibers <14mesh and <2 pm diameter formed during milling increased significantly to over 50% as a result of the acid pretreatment. This makes it possible to reduce the proportion of lyocell fibers in a cleaning cloth to significantly <25 wt .-%, according to the invention even under 20 wt.% And still obtain the required, described for example in US 8187422 property profiles.
Die erfindungsgemäßen schnell fibrillierenden Lyocellfasern können erfindungsgemäß zur Herstellung verschiedenster Produkte wie The fast-fibrillating lyocell fibers according to the invention can be used according to the invention for the production of a wide variety of products, such as
Wischtüchern, insbesondere Einweg-Wischtüchern, Papieren, insbesondere Filterpapieren und Papieren für technische Anwendungen wie Batterien, etc. eingesetzt werden. Diese und weitere Produkte sowie die dafür in Frage kommenden Herstellungsverfahren sind unter anderem in der WO 95/35399 beschrieben, auf die hiermit verwiesen wird und deren Offenbarung Wiping cloths, especially disposable wipes, papers, in particular filter papers and papers for technical applications such as batteries, etc. are used. These and other products as well as the manufacturing processes in question are described inter alia in WO 95/35399, to which reference is hereby made and the disclosure thereof
vollinhaltlich in die vorliegende Patentanmeldung übernommen wird. is fully incorporated into the present patent application.
Insbesondere können erfindungsgemäße Wischtücher nach grundsätzlich bekannten Verfahren aus den erfindungsgemäßen Fasern und Zellstoff hergestellt werden. In einer bevorzugten Ausführungsform erfolgt die In particular, wipes according to the invention can be prepared by basically known processes from the fibers and pulp according to the invention. In a preferred embodiment, the
Verfestigung durch Wasservernadelung. Solidification by water needling.
Gegenstand der vorliegenden Erfindung ist auch die Verwendung der oben beschriebenen erfindungsgemäßen Fasern zur Herstellung eines Wischtuchs, wobei das Wischtuch Zellstoff und 5 bis 20 Gew.-% fibrillierte Lyocellfasern enthält Der Zellstoff ist bevorzugt ein Papierzellstoff. The present invention also relates to the use of the inventive fibers described above for producing a wipe, wherein the wipe comprises pulp and 5 to 20 wt .-% fibrillated lyocell fibers. The pulp is preferably a paper pulp.
Im Folgenden wird die Erfindung anhand von Beispielen beschrieben. Die Erfindung ist jedoch ausdrücklich nicht auf diese Beispiele beschränkt, sondern umfasst auch alle anderen Ausführungsformen, die auf dem gleichen erfinderischen Konzept beruhen. In the following the invention will be described by way of examples. However, the invention is expressly not limited to these examples, but includes all other embodiments based on the same inventive concept.
Beispiele Examples
Beispiel 1 : Säurebehandlung Example 1: Acid treatment
Erfindungsgemäße schnell fibrillierende Lyocell-Fasern werden wie folgt hergestellt: Ein Lyocell-Faserstrang mit einem Einzelfasertiter von 1 ,7dtex wird mit verdünnter Schwefelsäure bei Raumtemperatur und einem Fast fibrillating lyocell fibers according to the invention are produced as follows: A lyocell fiber strand having a single fiber titer of 1.7 dtex is diluted with dilute sulfuric acid at room temperature and a
Flottenverhältnis von 1 :10 imprägniert und auf ca. 200% Feuchte abgepresst. Der imprägnierte Faserstrang wird in einem Labordämpfer für ca. 10min mit Wasserdampf unter Druck beaufschlagt, anschließend mit Wasser säurefrei gewaschen und getrocknet. Der trockene Faserstrang wird auf 5mm  Liquor ratio of 1: 10 impregnated and pressed to about 200% moisture. The impregnated fiber strand is subjected to steam in a laboratory damper for about 10 minutes under pressure, then washed free of acid with water and dried. The dry fiber strand becomes 5mm
Stapellänge geschnitten und der CSF Prüfung unterzogen.  Cut the staple length and undergo the CSF test.
Beispiel 2: Vergleich der Fibrillationsdynamik Example 2: Comparison of fibrillation dynamics
Die Fibrillationsneigung wird mittels einer CSF (Canadian Standard of Freeness) Prüfung gemäß TAPPI Standard T227 om-94 gemessen und der Fibrillationsquotient Q ermittelt. Verglichen wurden: The fibrillation tendency is measured by means of a CSF (Canadian Standard of Freeness) test according to TAPPI Standard T227 om-94 and the fibrillation quotient Q is determined. Compared:
A. handelsübliche unbehandelte 1 ,7 dtex/6mm Lyocell-Fasern, A. Commercially available untreated 1.7 dtex / 6 mm lyocell fibers,
kommerziell erhältlich als Tencel® von der Lenzing AG („Tencel®- Standard")  commercially available as Tencel® from Lenzing AG ("Tencel® standard")
B. Gemäß Beispiel 1 säurebehandelte Fasern („ Tencel® schnell fibrillierend") B. Acid-treated fibers according to Example 1 ("Tencel® fast fibrillating")
Fig. 1 zeigt die Abnahme des CSF-Wertes mit zunehmender Fig. 1 shows the decrease of the CSF value with increasing
Zerkleinerungszeit in der Meßvorrichtung. Es läßt sich gut erkennen, daß die säurebehandelten Fasern deutlich schneller fibrillieren als die unbehandelten. Dies bedeutet für die Praxis der kommerziellen Herstellung fibrillierter  Crushing time in the measuring device. It can be clearly seen that the acid-treated fibers fibrillate much faster than the untreated. This means more fibrillated for commercial production
Lyocellfasern einen erheblich geringeren Zeit- und Energieaufwand als bei Verwendung unbehandelter Lyocellfasern.  Lyocell fibers significantly less time and energy than when using untreated Lyocell fibers.
Tab. 1 zeigt die für die verschiedenen Proben ermittelten tcsF2oo-Werte und die daraus errechneten Q-Werte. Table 1 shows the tcsF2oo values determined for the various samples and the Q values calculated from them.
Tab. 1 : Beispiel 3: Vergleich der Eignung für Nasslegeverfahren Tab. 1: Example 3: Comparison of Suitability for Wetlaying Methods
Verglichen wurden die gleichen Faserproben wie in Beispiel 1 : The same fiber samples were compared as in Example 1:
Jeweils 1 %ige wässrige Fasersuspensionen beider Faserproben A und B wurden in einem Laborrefiner vom Typ Andritz R1 L bei einer Leistung von 500W vermählen, wobei sowohl der Energieverbrauch in kWh/to als auch die Dauer zur Erreichung eines Mahlgrades von CSF 200 (Canadian Standard of Freeness-Prüfung gemäß TAPPI Standard T227 om-94) ermittelt wurden. Die fibrillierende Lyocellfaser konnte im Vergleich zur Standard-Lyocellfaser in nur 50 % der Vermahlungsdauer mit weniger als 80% des Energieverbrauchs verarbeitet werden (siehe Tab. 2). Each 1% aqueous fiber suspensions of both fiber samples A and B were ground in a laboratory refiner Andritz R1 L at a power of 500W, both the energy consumption in kWh / to and the duration to achieve a degree of grinding of CSF 200 (Canadian Standard of Freeness test according to TAPPI Standard T227 om-94). The fibrillating lyocell fiber could be processed in less than 80% of the energy consumption compared to the standard lyocell fiber in only 50% of the milling time (see Table 2).
Tab. 2: Tab. 2:
Von 2000 ml dieser wurden in einem Blattbildner vom Typ Rapith Kothen Versuchsblätter hergestellt und REM-Aufnahmen dieser Versuchsblätter gemacht. Fig. 2 zeigt eine REM-Aufnahme des Blattes aus der Suspension von Probe B. 2000 ml of these were used to prepare test sheets in a Rapith Kothen sheet former and to take SEM images of these test sheets. FIG. 2 shows an SEM image of the leaf from the suspension of sample B. FIG.

Claims

Patentansprüche claims
1. Wischtuch, das Zellstoff und 5 bis 20 Gew.-% fibrillierte Lyocellfasern enthält, dadurch gekennzeichnet, dass die fibrillierten Lyocellfasern einen Fibrillationsquotienten Q von 20 oder größer aufweisen. 1. A wipe containing pulp and 5 to 20% by weight of fibrillated lyocell fibers, characterized in that the fibrillated lyocell fibers have a fibrillation quotient Q of 20 or greater.
2. Wischtuch gemäß Anspruch 1 , wobei der Zellstoff ein Papierzellstoff ist. A wipe according to claim 1, wherein the pulp is a paper pulp.
3. Fibrillierte Lyocellfasern, dadurch gekennzeichnet, dass sie einen Fibrillationsquotienten Q von 20 oder größer aufweisen und ihr Gehalt an Mikrofasem mit einer Feinheit von kleiner 14 mesh und einem Durchmesser von kleiner 2 pm mindestens 50% beträgt. 3. fibrillated lyocell fibers, characterized in that they have a Fibrillationsquotienten Q of 20 or greater and their content of microfibers with a fineness of less than 14 mesh and a diameter of less than 2 pm is at least 50%.
4. Verwendung der Fasern nach Anspruch 3 zur Herstellung eines Wischtuchs, dadurch gekennzeichnet, dass das Wischtuch Zellstoff und 5 bis 20 Gew.-% fibrillierte Lyocellfasern enthält.  4. Use of the fibers according to claim 3 for the production of a wipe, characterized in that the wipe contains pulp and 5 to 20 wt .-% fibrillated lyocell fibers.
5. Verwendung gemäß Anspruch 4, wobei der Zellstoff ein Papierzellstoff ist.  Use according to claim 4, wherein the pulp is a paper pulp.
6. Verwendung der fibrillierten Lyocellfasern nach Anspruch 3 in Nasslegeverfahren.  6. Use of the fibrillated lyocell fibers according to claim 3 in wet-laying process.
7. Verwendung nach Anspruch 6 in Mischung der fibrillierten Lyocellfasern mit Papierzellstoff mit einem Lyocellfaser-Anteil zwischen 5 - 20 Gew.%.  7. Use according to claim 6 in a mixture of the fibrillated lyocell fibers with paper pulp with a lyocell fiber content between 5 - 20 wt.%.
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