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WO2013026528A1 - Aqueous dispersion for treating natural fibers and method for treating natural fibers - Google Patents

Aqueous dispersion for treating natural fibers and method for treating natural fibers Download PDF

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Publication number
WO2013026528A1
WO2013026528A1 PCT/EP2012/003340 EP2012003340W WO2013026528A1 WO 2013026528 A1 WO2013026528 A1 WO 2013026528A1 EP 2012003340 W EP2012003340 W EP 2012003340W WO 2013026528 A1 WO2013026528 A1 WO 2013026528A1
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WO
WIPO (PCT)
Prior art keywords
natural fibers
aqueous dispersion
fibers
pigments
water
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.)
Ceased
Application number
PCT/EP2012/003340
Other languages
German (de)
French (fr)
Inventor
Martin Sonntag
Katja Fischer
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.)
Rehau Automotive SE and Co KG
Original Assignee
Rehau AG and Co
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 Rehau AG and Co filed Critical Rehau AG and Co
Priority to EP12745633.3A priority Critical patent/EP2744939A1/en
Publication of WO2013026528A1 publication Critical patent/WO2013026528A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00—Macromolecular compounds derived from lignocellulosic materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/045—Reinforcing macromolecular compounds with loose or coherent fibrous material with vegetable or animal fibrous material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06—Waxes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/22—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using vat dyestuffs including indigo
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/22—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using vat dyestuffs including indigo
    • D06P1/24—Anthraquinone dyes or anthracene nucleus containing vat dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
    • D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
    • D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
    • D06P1/56—Condensation products or precondensation products prepared with aldehydes
    • D06P1/58—Condensation products or precondensation products prepared with aldehydes together with other synthetic macromolecular substances
    • 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
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • 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
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • D21H11/20—Chemically or biochemically modified fibres
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
    • D21H17/74—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic and inorganic material
    • 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
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/16—Sizing or water-repelling agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

Definitions

  • Aqueous dispersion for the treatment of natural fibers and
  • the present invention relates to an aqueous dispersion for treating natural fibers and to a method of treating natural fibers.
  • the invention relates to a composite material of a thermoplastically processable polymer material and natural fibers and an article of the composite material.
  • thermoplastically processable polymer material and natural fibers, in particular wood fibers, see due to their favorable properties in the meantime a very wide use.
  • Articles made of this composite material are used as floor coverings, cladding, construction elements, in horticulture, as fences and in garden furniture.
  • Polymeric material and natural fibers in general is that the natural fibers absorb water to some extent, swell and are susceptible to attack by microorganisms such as fungi, algae, mosses and lichens.
  • the object of the invention is achieved by an aqueous dispersion for the treatment of natural fibers according to claim 1.
  • the aqueous dispersion for the treatment of natural fibers contains a water-soluble or dispersible, adhering to a natural fiber hydrophobing agent, and a pigment preparation which is dispersed in water, and water.
  • aqueous dispersion of the type described is particularly favorable for the coating of natural fibers with the hydrophobizing agent, with simultaneous coloring of the natural fibers with the pigment preparation. It has been found in the context of the invention to be very advantageous if the water-soluble or dispersible, adhering to a natural fiber hydrophobing agent is selected from an epoxy resin, a melamine resin, a urea-based resin, a low molecular weight wax, a silicone resin, a water glass, an ethyl vinyl acrylate and a ethyl methacrylate.
  • water repellents are particularly well suited to coat the natural fibers, in particular the wood fibers, and thus to minimize the water absorption of natural fibers, in particular of wood fibers.
  • inorganic and / or organic pigments are suitable as water-dispersible pigment preparations.
  • Inorganic pigments in this context include white pigments, black pigments and colored pigments.
  • Organic pigments may include anthraquinone pigments and triaryl carbonium pigments.
  • the above-mentioned pigments are very well suited in the context of the present invention to color the natural fibers, in particular the wood fibers.
  • the object of the invention to provide a method for the treatment of natural fibers is achieved with claim 4.
  • the process according to the invention for the treatment of natural fibers comprises the steps of providing natural fibers
  • natural fibers which are preferably wood fibers.
  • the wood fibers may be derived from softwoods such as spruce, pine, larch, birch, willow, poplar or linden or mixtures thereof, or from hardwoods such as beech, oak, ash and their mixtures as well as mixtures of natural fibers of softwoods and hardwoods.
  • the fibers used should have an average length of 80 to 1000 m
  • the moisture of the natural fibers to be treated should be between 0.5 and 10 wt .-%.
  • the fiber width of natural fibers is about 30 to 40 ⁇ (microns), making them particularly suitable for the pretreatment process.
  • the pretreatment itself can be done in different ways.
  • the aqueous dispersion may be added to the natural fibers in a continuous process, for example, when the natural fibers are agitated in a screw conveyor, the aqueous dispersion then being sprayed, for example. In this case, it can be specified very precisely which proportion of aqueous dispersion is added to the amount of natural fibers.
  • the aqueous dispersion can be added to the natural fibers, for example in a mixer.
  • a predetermined amount of natural fibers is mixed with a correspondingly determined amount of aqueous dispersion and the mixture is distributed as homogeneously as possible by suitable mixing technique.
  • the pretreated natural fibers may, for example, pass through a drying oven, in which they release water using elevated temperature, if necessary assisted by a treatment with predried air and / or application of a reduced pressure, until the desired residual moisture is established.
  • a temperature for drying the fibers in a drying oven a temperature is preferably selected between 100 ° C and 200 ° C, in this case, the curing / drying of the resin / hydrophobizing agent on the natural fibers and / or melting of the low molecular weight waxes, whereby the natural fibers are then impregnated become.
  • the content of pigment after the re-drying of the natural fibers is ideally 0.5 to 6% by weight.
  • the content of hydrophobing agent should be about 1 to 15 wt .-% in relation to the dried natural fiber amount.
  • the invention also includes a drying step before the natural fibers are brought into contact with the aqueous dispersion.
  • a drying step before the natural fibers are brought into contact with the aqueous dispersion.
  • the composite material is chosen so that the proportion of natural fibers in the composite material 20 to 80 wt .-%, preferably about 55 wt .-%, is.
  • the natural fibers are advantageously selected so that they have a length of 80 to 1000 ⁇ (microns). Fibers with an average length of about 600 pm (microns) are best suited.
  • Suitable natural fibers in the context of the present invention are very well fibers of wood. In principle, all conifers and hardwoods are suitable for this purpose.
  • fibers of spruce, pine, larch, birch, sage, poplar, linden, and their mixtures, suitable are fibers of spruce, pine, larch, birch, sage, poplar, linden, and their mixtures, suitable.
  • a composite material of a thermoplastically processable polymer material and natural fibers shows a water absorption which is ⁇ 5% by weight in a 28-day water storage based on DIN EN 317 of a surface-brushed test specimen and / or Color change of the surface of the specimen according to a Xeno test (4,500 h Weatherometer Ci 5000 according to ISO 4892-2) Delta E ⁇ 4 and / or the water absorption in accordance with DIN EN 317 in a multiple repetition of the 28-day water storage after each Re-drying of the specimen to constant weight by at least 40% compared to a composite material whose natural fibers are not treated, is reduced.
  • the color change of the composite material according to the present invention is according to gray scale DIN EN ISO 105 A02 4-5.
  • Such a composite material made of a thermoplastically processable polymer material and pretreated with an aqueous dispersion of natural fibers thus shows a very low tendency for water absorption and only a negligible color change in an outdoor use.
  • thermoplastically processable polymer material all polymer materials which are thermoplastically processable are suitable as thermoplastically processable polymer material.
  • polypropylene PP
  • PE polyethylene
  • PB polybutylene
  • PVC polyvinyl chloride
  • PS polystyrene
  • ABS acrylonitrile-butadiene-styrene
  • An article of the composite material in particular an article made of a plastic-wood fiber composite material, as described in claim 10 and solves the object of the invention is characterized high quality, durable and in terms of infestation by fungi, algae, lichens, mosses and others Protected microorganisms and does not change its color outdoors or only insignificantly.
  • Articles made of the composite material find a variety of applications as patio / plank flooring, as a cladding, as a construction material and in the furniture sector.
  • the batch is then dried in a circulating air drying oven at 90 ° C. for 16 h (hours).
  • the wood fibers pretreated with the aqueous dispersion are then processed on a ZSK 25 compounding extruder with polypropylene as thermoplastically processable polymer material to form a plastic-wood fiber composite material (WPC, wood-plastic composite).
  • WPC plastic-wood fiber composite material
  • Test specimens are made of the plastic-wood fiber composite material to investigate the material properties by injection molding. The surface of the specimens is brushed or sanded to expose the wood fibers, then the tests are initiated immediately.
  • the resulting composite material consists of 60% by weight of natural fibers, 31% by weight of polypropylene, 1.5% by weight of pigments, 4% by weight of hydrophobing agent, 2% by weight of adhesion promoter and 2.5% by weight. % Additives and lubricants. test results
  • the color change Delta E was 1, 4.
  • the color change according to the gray scale according to DIN EN ISO 105 A02 was 4 - 5.
  • FIG. 2 is a graph for water absorption of a test plate made of a wood-plastic composite (WPC) containing untreated wood fibers;
  • WPC wood-plastic composite
  • FIG. 3 is a graph for water absorption of a test plate made of a wood-plastic composite (WPC), which contains wood fibers treated according to the invention.
  • FIG. 1 schematically shows a cross section through an article 1 made of a thermoplastically processable polymer material 2 and natural fibers 3.
  • Item size and natural fiber size and pigment particle size are not to scale, but freely chosen to illustrate the principle of the invention.
  • the natural fibers 3 are embedded in the thermoplastically processable polymer material 2.
  • the natural fibers 3 are coated by the pretreatment with the aqueous dispersion with a hydrophobing agent 4, which is connected to the fiber surface of the natural fibers 3 and adheres there.
  • pigment particles 5 are distributed, which give the natural fiber 3 color.
  • Pigment particles 5 can also - this is not shown in FIG. 1 - penetrate superficially into the pores of the natural fiber 3 and be bound therein.
  • the article 1 of the thermoplastically processable polymer material 2 and the natural fibers 3, on which water repellent 4 adheres with pigment particles 5, has a surface 6, which may be structured, in particular by a brushing process may have a Bürst Scheme ist.
  • Fig. 2 shows a graph for water absorption of a test plate from a wood-plastic composite (WPC) containing untreated wood fibers.
  • WPC wood-plastic composite
  • Fig. 3 shows a graph for water absorption of a test plate made of a wood-plastic composite (WPC) containing wood fibers treated according to the invention.
  • WPC wood-plastic composite
  • the wood fibers were pretreated with a melamine based water repellent. Compared to the untreated fiber, the water absorption after repeated storage and re-drying to constant weight (which was carried out at 80 ° C. in a circulating air oven) is significantly reduced compared to untreated wood fiber.
  • thermoplastically processable polymer material 3 natural fiber

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Biochemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Wood Science & Technology (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to an aqueous dispersion for treating natural fibers (3), and to a method for treating natural fibers (3). According to the invention, the aqueous dispersion for treating natural fibers (3), in particular wood fibers, contains a hydrophobic agent (4), which is water soluble or water dispersible and adheres to a natural fiber (3), a water dispersible pigment preparation, and water. The method for treating natural fibers (3) comprises the following steps: providing natural fibers (3), providing an aqueous dispersion, and bringing the natural fibers (3) in contact with the aqueous dispersion.

Description

Wässrige Dispersion zur Behandlung von Naturfasern und  Aqueous dispersion for the treatment of natural fibers and

Verfahren zur Behandlung von Naturfasern  Process for the treatment of natural fibers

Die vorliegende Erfindung betrifft eine wässrige Dispersion zur Behandlung von Naturfasern und ein Verfahren zur Behandlung von Naturfasern. The present invention relates to an aqueous dispersion for treating natural fibers and to a method of treating natural fibers.

Darüber hinaus betrifft die Erfindung einen Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern sowie einen Gegenstand aus dem Verbundwerkstoff. In addition, the invention relates to a composite material of a thermoplastically processable polymer material and natural fibers and an article of the composite material.

Verbundwerkstoffe aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern, insbesondere Holzfasern, finden aufgrund ihrer günstigen Eigenschaften inzwi- sehen eine sehr breite Verwendung. Composite materials of a thermoplastically processable polymer material and natural fibers, in particular wood fibers, see due to their favorable properties in the meantime a very wide use.

Gegenstände aus diesem Verbundwerkstoff sind als Bodenbeplankungen, Verkleidungen, Konstruktionselemente, im Gartenbau, als Zaunanlagen und im Gartenmöbelbau im Einsatz. Articles made of this composite material are used as floor coverings, cladding, construction elements, in horticulture, as fences and in garden furniture.

Nachteilig an diesem Verbundwerkstoff aus einem thermoplastisch verarbeitbaren A disadvantage of this composite material from a thermoplastically processable

Polymermaterial und Naturfasern ist im Allgemeinen, dass die Naturfasern bis zu einem gewissen Grad Wasser aufnehmen, dabei quellen und anfällig sind für den Angriff von Mikroorganismen, wie beispielsweise Pilzen, Algen, Moosen und Flechten. Polymeric material and natural fibers in general is that the natural fibers absorb water to some extent, swell and are susceptible to attack by microorganisms such as fungi, algae, mosses and lichens.

Ein weiterer Nachteil wird darin gesehen, dass die Naturfasern im Außeneinsatz unter dem Einfluss des UV-Anteils des Lichts über die Zeit ihre Farbe verändern, was in vielen Anwendungen ungewollt ist. Aufgabe der vorliegenden Erfindung ist es also, eine wässrige Dispersion zur Behandlung von Naturfasern anzugeben, mit der die oben aufgezeigten Probleme überwunden werden können, und ein Verfahren anzugeben, wie die Naturfasern zu behandeln sind. Eine weitere Aufgabe der Erfindung ist es, einen Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern anzugeben, der in Bezug auf die oben geschilderten Nachteile vorteilhaft weiterentwickelt ist. Es ist weiterhin Aufgabe der vorliegenden Erfindung, einen Gegenstand aus dem Verbundwerkstoff anzugeben. Another disadvantage is seen in the fact that the natural fibers change their color in the field under the influence of the UV component of the light over time, which is undesirable in many applications. It is therefore an object of the present invention to provide an aqueous dispersion for the treatment of natural fibers, with which the problems indicated above can be overcome, and to provide a method of treating the natural fibers. Another object of the invention is to provide a composite material of a thermoplastically processable polymer material and natural fibers, which is advantageously developed with respect to the disadvantages described above. It is a further object of the present invention to provide an article of the composite material.

Die Aufgabe der Erfindung wird gelöst durch eine wässrige Dispersion zur Behandlung von Naturfasern gemäß Anspruch 1. The object of the invention is achieved by an aqueous dispersion for the treatment of natural fibers according to claim 1.

Es hat sich als vorteilhaft erwiesen, wenn die wässrige Dispersion zur Behandlung von Naturfasern, insbesondere von Holzfasern, ein in Wasser lösliches oder dispergierbares, auf einer Naturfaser haftendendes Hydrophobierungsmittel, und eine Pigmentzubereitung enthält, die in Wasser dispergiert ist, sowie Wasser. It has proved to be advantageous if the aqueous dispersion for the treatment of natural fibers, in particular of wood fibers, contains a water-soluble or dispersible, adhering to a natural fiber hydrophobing agent, and a pigment preparation which is dispersed in water, and water.

Eine wässrige Dispersion der geschilderten Art ist besonders günstig für die Beschichtung von Naturfasern mit dem Hydrophobierungsmittel, unter gleichzeitiger Einfärbung der Naturfasern mit der Pigmentzubereitung. Es hat sich im Erfindungszusammenhang als sehr vorteilhaft herausgestellt, wenn das in Wasser lösliche oder dispergierbare, auf einer Naturfaser haftendende Hydrophobierungsmittel ausgewählt ist aus einem Epoxidharz, einem Melaminharz, einem harnstoffbasierenden Harz, einem niedermolekularen Wachs, einem Silikonharz, einem Wasserglas, einem Ethylvinylacrylat und einem Ethylmethacrylat. An aqueous dispersion of the type described is particularly favorable for the coating of natural fibers with the hydrophobizing agent, with simultaneous coloring of the natural fibers with the pigment preparation. It has been found in the context of the invention to be very advantageous if the water-soluble or dispersible, adhering to a natural fiber hydrophobing agent is selected from an epoxy resin, a melamine resin, a urea-based resin, a low molecular weight wax, a silicone resin, a water glass, an ethyl vinyl acrylate and a ethyl methacrylate.

Die vorstehend bezeichneten Hydrophobierungsmittel sind besonders gut geeignet, die Naturfasern, insbesondere die Holzfasern, zu beschichten und damit die Wasseraufnahme der Naturfasern, insbesondere der Holzfasern, zu minimieren. Als in Wasser dispergierbare Pigmentzubereitungen eignen sich im Rahmen der Erfindung anorganische und / oder organische Pigmente. The above-described water repellents are particularly well suited to coat the natural fibers, in particular the wood fibers, and thus to minimize the water absorption of natural fibers, in particular of wood fibers. In the context of the invention, inorganic and / or organic pigments are suitable as water-dispersible pigment preparations.

Anorganische Pigmente umfassen in diesem Zusammenhang Weißpigmente, Schwarzpigmente und Buntpigmente. Organische Pigmente können dabei Anthrachinon-Pigmente und Triarylcarbonium-Pigmente umfassen. Die vorstehend genannten Pigmente sind im Rahmen der vorliegenden Erfindung sehr gut geeignet, die Naturfasern, insbesondere die Holzfasern, einzufärben. Die Aufgabe der Erfindung, ein Verfahren zur Behandlung von Naturfasern anzugeben, wird mit Anspruch 4 gelöst. Inorganic pigments in this context include white pigments, black pigments and colored pigments. Organic pigments may include anthraquinone pigments and triaryl carbonium pigments. The above-mentioned pigments are very well suited in the context of the present invention to color the natural fibers, in particular the wood fibers. The object of the invention to provide a method for the treatment of natural fibers is achieved with claim 4.

Das erfindungsgemäße Verfahren zur Behandlung von Naturfasern umfasst die Schritte · Bereitstellen von Naturfasern The process according to the invention for the treatment of natural fibers comprises the steps of providing natural fibers

• Bereitstellen einer wässrigen Dispersion, wie sie vorstehend beschrieben ist, Providing an aqueous dispersion as described above

• Inkontaktbringen der Naturfasern mit der wässrigen Dispersion. • contacting the natural fibers with the aqueous dispersion.

Es hat sich hierbei als günstig erwiesen, wenn Naturfasern eingesetzt werden, die bevor- zugt Holzfasern sind. Die Holzfasern können von Weichhölzern, wie beispielsweise Fichte, Kiefer, Lärche, Birke, Weide, Pappel oder Linde oder deren Mischungen stammen, oder von Harthölzern, wie beispielsweise Buche, Eiche, Esche und deren Mischungen sowie auch Mischungen von Naturfasern von Weichhölzern und Harthölzern. Die verwendeten Fasern sollen dabei eine durchschnittliche Länge von 80 bis 1000 mIt has proved to be advantageous here if natural fibers are used, which are preferably wood fibers. The wood fibers may be derived from softwoods such as spruce, pine, larch, birch, willow, poplar or linden or mixtures thereof, or from hardwoods such as beech, oak, ash and their mixtures as well as mixtures of natural fibers of softwoods and hardwoods. The fibers used should have an average length of 80 to 1000 m

(Mikrometer) aufweisen. Im Rahmen der Erfindung hat sich herausgestellt, dass am besten geeignet sind Fasern von etwa 600 μιτι (Mikrometer) Länge. (Micrometers). In the context of the invention, it has been found that fibers of approximately 600 μιτι (microns) in length are most suitable.

Die Feuchtigkeit der zu behandelnden Naturfasern soll dabei zwischen 0,5 und 10 Gew.-% liegen. Die Faserbreite der Naturfasern beträgt etwa 30 bis 40 μιτι (Mikrometer), wodurch sie ganz besonders für den Vorbehandlungsprozess geeignet sind. Die Vorbehandlung selbst kann dabei auf verschiedenen Wegen erfolgen. The moisture of the natural fibers to be treated should be between 0.5 and 10 wt .-%. The fiber width of natural fibers is about 30 to 40 μιτι (microns), making them particularly suitable for the pretreatment process. The pretreatment itself can be done in different ways.

A. Kontinuierlicher Vorbehandlungsprozess A. Continuous pretreatment process

Die wässrige Dispersion kann zu den Naturfasern in einem kontinuierlichen Prozess hinzugegeben werden, beispielsweise wenn die Naturfasern in einem Schneckenförderer bewegt werden, wobei die wässrige Dispersion dann beispielsweise aufgesprüht wird. Hierbei kann sehr genau vorgegeben werden, welcher Anteil an wässriger Dispersion der Menge an Naturfasern zugegeben wird. The aqueous dispersion may be added to the natural fibers in a continuous process, for example, when the natural fibers are agitated in a screw conveyor, the aqueous dispersion then being sprayed, for example. In this case, it can be specified very precisely which proportion of aqueous dispersion is added to the amount of natural fibers.

B. Diskontinuierlicher Vorbehandlungprozess B. Discontinuous pretreatment process

In einem diskontinuierlichen Prozess kann die wässrige Dispersion den Naturfasern beispielsweise in einem Mischer zugegeben werden. In a batch process, the aqueous dispersion can be added to the natural fibers, for example in a mixer.

Hierbei wird eine vorgegebene Menge Naturfasern mit einer entsprechend bestimmten Menge an wässriger Dispersion versetzt und die Mischung durch geeignete Mischtechnik möglichst homogen verteilt. In this case, a predetermined amount of natural fibers is mixed with a correspondingly determined amount of aqueous dispersion and the mixture is distributed as homogeneously as possible by suitable mixing technique.

Auch hier ist es möglich, sehr exakt der Menge an Naturfasern eine Menge an wässriger Dispersion zur Vorbehandlung zuzusetzen. Again, it is possible to add very accurately to the amount of natural fibers, an amount of aqueous dispersion for pretreatment.

Es hat sich im Rahmen der Erfindung weiterhin herausgestellt, dass es sehr günstig ist, die mit der wässrigen Dispersion versetzten Naturfasern nach dem Inkontaktbringen einem Trocknungsprozess zu unterziehen, um die Naturfasern bis zu einer vorbestimmten Restfeuchte zu trocknen. It has further been found within the scope of the invention that it is very favorable to subject the natural fibers, mixed with the aqueous dispersion, after the contacting to a drying process in order to dry the natural fibers to a predetermined residual moisture content.

Dies ist entscheidend für die Weiterverarbeitung der mit der wässrigen Dispersion vorbehandelten Naturfasern zu einem Verbundwerkstoff, der weiterhin ein thermoplastisch verarbeitbares Polymermaterial enthält. Hierzu ist es notwendig, dass die Restfeuchte der, wie vorstehend beschrieben, vorbehandelten Naturfasern unter 1 Gew.-% gebracht wird. This is crucial for the further processing of the pretreated with the aqueous dispersion of natural fibers into a composite material, which further contains a thermoplastically processable polymer material. For this purpose, it is necessary that the residual moisture content of the pretreated natural fibers, as described above, is brought below 1 wt .-%.

Hierzu können die vorbehandelten Naturfasern beispielsweise einen Trockenofen durchlaufen, in dem sie unter Anwendung erhöhter Temperatur, ggf. unterstützt durch eine Behand- lung mit vorgetrockneter Luft und / oder Anwendung eines Unterdrucks, Wasser abgeben, bis die gewünschte Restfeuchte eingestellt ist. For this purpose, the pretreated natural fibers may, for example, pass through a drying oven, in which they release water using elevated temperature, if necessary assisted by a treatment with predried air and / or application of a reduced pressure, until the desired residual moisture is established.

Es hat sich in diesem Zusammenhang erfindungsgemäß als günstig erwiesen, wenn der Feuchtegehalt der mit der wässrigen Dispersion vorbehandelten Naturfasern unmittelbar nach der Vorbehandlung 15 Gew.-% möglichst nicht überschreitet. Als Temperatur zur Trocknung der Fasern in einem Trockenofen wird eine Temperatur vorzugsweise zwischen 100 °C und 200 °C gewählt, hierbei erfolgt das Aushärten / Trocknen des Harzes / Hydrophobierungsmittels auf den Naturfasern und / oder ein Aufschmelzen der niedermolekularen Wachse, wodurch die Naturfasern dann imprägniert werden. In this context, it has proved favorable in accordance with the invention if the moisture content of the natural fibers pretreated with the aqueous dispersion does not exceed 15% by weight immediately after the pretreatment. As the temperature for drying the fibers in a drying oven, a temperature is preferably selected between 100 ° C and 200 ° C, in this case, the curing / drying of the resin / hydrophobizing agent on the natural fibers and / or melting of the low molecular weight waxes, whereby the natural fibers are then impregnated become.

Als günstig hat sich im Rahmen der Erfindung erweisen, wenn der Gehalt an Pigment nach der Rücktrocknung der Naturfasern idealerweise 0,5 bis 6 Gew.-% beträgt. In the context of the invention, it has proved favorable if the content of pigment after the re-drying of the natural fibers is ideally 0.5 to 6% by weight.

Der Gehalt an Hydrophobierungsmittel soll in Bezug auf die getrocknete Naturfasermenge etwa 1 bis 15 Gew.-% betragen. The content of hydrophobing agent should be about 1 to 15 wt .-% in relation to the dried natural fiber amount.

Die Erfindung umfasst in einer vorteilhaften Weiterbildung auch einen Trocknungsschritt vor dem Inkontaktbringen der Naturfasern mit der wässrigen Dispersion. Durch das Vortrocknen der Naturfasern vor dem Inkontaktbringen mit der wässrigen Dispersion im Rahmen des Trocknungsschrittes werden die Naturfasern vorteilhaft vorkonditioniert, so dass sie beim Inkontaktbringen mit der wässrigen Dispersion diese besonders bevorzugt aufnehmen. Hierdurch können die Naturfasern sehr vorteilhaft schnell beschichtet und eingefärbt werden. In an advantageous development, the invention also includes a drying step before the natural fibers are brought into contact with the aqueous dispersion. By predrying the natural fibers prior to contacting with the aqueous dispersion in the course of the drying step, the natural fibers are advantageously preconditioned so that when they are brought into contact with the aqueous dispersion they are particularly preferably absorbed. As a result, the natural fibers can be very quickly coated and dyed very advantageous.

Die Lösung der Aufgabe, einen Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern anzugeben, ist mit Anspruch 8 gelöst. The solution of the problem to provide a composite material of a thermoplastically processable polymer material and natural fibers, is solved with claim 8.

Es wurde im Rahmen der Erfindung erkannt, dass ein Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern, die mit einer wässrigen Dispersion gemäß vorstehender Beschreibung behandelt sind, die Nachteile des Standes der Technik überwindet. It has been recognized within the scope of the invention that a composite material of a thermoplastically processable polymer material and natural fibers, which are treated with an aqueous dispersion as described above, overcomes the disadvantages of the prior art.

Es hat sich dabei als günstig erweisen, wenn der Verbundwerkstoff so gewählt wird, dass der Anteil der Naturfasern im Verbundwerkstoff 20 bis 80 Gew.-%, vorzugsweise etwa 55 Gew.-%, beträgt. It has proved to be advantageous if the composite material is chosen so that the proportion of natural fibers in the composite material 20 to 80 wt .-%, preferably about 55 wt .-%, is.

Die Naturfasern werden vorteilhaft so ausgewählt, dass sie eine Länge von 80 bis 1000 μιτι (Mikrometer) aufweisen. Am besten sind Fasern mit einer durchschnittlichen Länge von etwa 600 pm (Mikrometer) geeignet. The natural fibers are advantageously selected so that they have a length of 80 to 1000 μιτι (microns). Fibers with an average length of about 600 pm (microns) are best suited.

Als Naturfasern eignen sich im Rahmen der vorliegenden Erfindung sehr gut Fasern aus Holz. Hierzu sind prinzipiell alle Nadel- und Laubhölzer geeignet. Suitable natural fibers in the context of the present invention are very well fibers of wood. In principle, all conifers and hardwoods are suitable for this purpose.

Besonders gut sind Fasern der Fichte, Kiefer, Lärche, Birke, Weise, Pappel, Linde, sowie deren Mischungen, geeignet.  Especially good are fibers of spruce, pine, larch, birch, sage, poplar, linden, and their mixtures, suitable.

Auch Harthölzer sind geeignet, umfassend Buche, Eiche, Esche, und deren Mischungen. Insbesondere wurde im Rahmen der Erfindung gefunden, dass ein Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und Naturfasern eine Wasseraufnahme zeigt, die bei einer 28-tägigen Wasserlagerung in Anlehnung an DIN EN 317 eines oberflächengebürsteten Probekörpers < 5 Gew.-% beträgt und / oder dass die Farbveränderung der Oberfläche des Probekörpers nach einem Xeno-Test (4.500 h Weatherometer Ci 5000 nach ISO 4892-2) Delta E < 4 beträgt und / oder die Wasseraufnahme in Anlehnung an DIN EN 317 bei einer auch mehrfachen Wiederholung der 28-tägigen Wasserlagerung nach jeweiliger Rücktrocknung des Probekörpers bis zur Gewichtskonstanz um mindestens 40 % gegenüber einem Verbundwerkstoff, dessen Naturfasern nicht behandelt sind, reduziert ist.  Also hardwoods are suitable, including beech, oak, ash, and their mixtures. In particular, it has been found within the scope of the invention that a composite material of a thermoplastically processable polymer material and natural fibers shows a water absorption which is <5% by weight in a 28-day water storage based on DIN EN 317 of a surface-brushed test specimen and / or Color change of the surface of the specimen according to a Xeno test (4,500 h Weatherometer Ci 5000 according to ISO 4892-2) Delta E <4 and / or the water absorption in accordance with DIN EN 317 in a multiple repetition of the 28-day water storage after each Re-drying of the specimen to constant weight by at least 40% compared to a composite material whose natural fibers are not treated, is reduced.

Die Farbveränderung des Verbundwerkstoffs gemäß vorliegender Erfindung beträgt nach Graumaßstab DIN EN ISO 105 A02 4 - 5. The color change of the composite material according to the present invention is according to gray scale DIN EN ISO 105 A02 4-5.

Ein derartiger Verbundwerkstoff aus einem thermoplastisch verarbeitbaren Polymermaterial und aus mit einer wässrigen Dispersion vorbehandelten Naturfasern zeigt somit eine sehr geringe Tendenz zur Wasseraufnahme und nur eine vernachlässigbare Farbveränderung bei einem Außeneinsatz. Such a composite material made of a thermoplastically processable polymer material and pretreated with an aqueous dispersion of natural fibers thus shows a very low tendency for water absorption and only a negligible color change in an outdoor use.

In der folgenden Tabelle 1 sind die Messwerte vergleichend für ein Wood-Plastic- Composite (WPC) mit unbehandelten Holzfasern und für ein Wood-Plastic-Composite (WPC) mit entsprechend der vorliegenden Erfindung behandelten Holzfasern aufgelistet.

Figure imgf000009_0001
In the following Table 1, the measured values are listed comparatively for a wood-plastic composite (WPC) with untreated wood fibers and for a wood-plastic composite (WPC) with wood fibers treated according to the present invention.
Figure imgf000009_0001

Tabelle 1 Table 1

Durch die Verringerung der Wasseraufnahme der Naturfasern, die durch die Vorbehand- lung mit der wässrigen Dispersion verursacht ist, werden die Wachstumsbedingungen für Pilze, Algen, Flechten, Moose und andere Mikroorganismen verschlechtert. By reducing the water absorption of the natural fibers caused by the pretreatment with the aqueous dispersion, the growth conditions of fungi, algae, lichens, mosses and other microorganisms are deteriorated.

Dadurch kann auf den Einsatz von chemischen Zusatzstoffen, z.B. Bioziden, zur Verhinderung des biologischen Befalls des Verbundwerkstoffs durch die vorstehend genannten Mik- roorganismen verzichtet werden. This may indicate the use of chemical additives, e.g. Biocides, to prevent the biological attack of the composite material by the aforementioned microorganisms are omitted.

Hierdurch ist die Langzeitstabilität und Dauerhaftigkeit der Naturfasern im Verbundwerkstoff - und dadurch auch der Verbundwerkstoff selbst - gegenüber dem Stand der Technik wesentlich verbessert. As a result, the long-term stability and durability of natural fibers in the composite material - and thereby also the composite itself - over the prior art significantly improved.

Als thermoplastisch verarbeitbares Polymermaterial eignen sich im Zusammenhang mit der vorstehend beschriebenen Erfindung alle Polymermaterialien, die thermoplastisch verarbeitbar sind. In the context of the invention described above, all polymer materials which are thermoplastically processable are suitable as thermoplastically processable polymer material.

Besonders bevorzugt sind hierbei: Polypropylen (PP), Polyethylen (PE), Polybutylen (PB), Polyvinylchlorid (PVC), Polystyrol (PS), Acrylnitril-Butadien-Styrol (ABS), Polyester, Polyamide, Polyurethane, Polyether und thermoplastische Elastomere. Ein Gegenstand aus dem Verbundwerkstoff, insbesondere ein Gegenstand aus einem Kunststoff-Holzfaser-Verbundwerkstoff, wie er in Anspruch 10 beschrieben ist und die Aufgabe der Erfindung löst, ist dadurch hochwertig, langlebig und hinsichtlich des Befalls durch Pilze, Algen, Flechten, Moose und andere Mikroorganismen geschützt und verändert im Außeneinsatz seine Farbe nicht oder nur unwesentlich. Particularly preferred are: polypropylene (PP), polyethylene (PE), polybutylene (PB), polyvinyl chloride (PVC), polystyrene (PS), acrylonitrile-butadiene-styrene (ABS), polyesters, polyamides, polyurethanes, polyethers and thermoplastic elastomers. An article of the composite material, in particular an article made of a plastic-wood fiber composite material, as described in claim 10 and solves the object of the invention is characterized high quality, durable and in terms of infestation by fungi, algae, lichens, mosses and others Protected microorganisms and does not change its color outdoors or only insignificantly.

Gegenstände aus dem Verbundwerkstoff, insbesondere Gegenstände aus einem Kunststoff-Holzfaser-Verbundwerkstoff, finden vielfältige Anwendung als Terrassen- / Dielenbelag, als Verkleidung, als Konstruktionsmaterial und im Möbelbereich. Articles made of the composite material, in particular articles made of a plastic-wood fiber composite material, find a variety of applications as patio / plank flooring, as a cladding, as a construction material and in the furniture sector.

Im Folgenden ist ein Ausführungsbeispiel der vorliegenden Erfindung im Detail beschrieben. Hereinafter, an embodiment of the present invention will be described in detail.

In einem beheizbaren Schnellmischer werden Weichholzfasern mit einer mittleren Faser- länger von 500 pm (Mikrometer) vorgelegt. Unter Rühren werden bei Raumtemperatur 200 ml (Milliliter) einer wässrigen Dispersion aus einem in Wasser löslichen oder dispergierbaren, auf einer Naturfaser haftendenden Hydrophobierungsmittel und einer in Wasser dispergierbaren Pigmentzubereitung über einen Zeitraum von 5 min zudosiert. Der Ansatz wird nach Zugabe der Dispersion noch weitere 5 min im Mischer gerührt, um die wässrige Dispersion gleichmäßig auf der Fasermenge zu verteilen. In a heated high-speed mixer softwood fibers with a mean fiber length of 500 pm (microns) are presented. While stirring, 200 ml (milliliters) of an aqueous dispersion of a water-soluble or dispersible, natural-fiber-based hydrophobing agent and a water-dispersible pigment preparation are metered in over a period of 5 minutes. The mixture is stirred for a further 5 minutes in the mixer after addition of the dispersion in order to distribute the aqueous dispersion uniformly on the amount of fiber.

Anschließend wird der Ansatz im Umlufttrockenschrank bei 90 °C für 16 h (Stunden) getrocknet. Die mit der wässrigen Dispersion vorbehandelten Holzfasern werden anschlie- ßend auf einem ZSK 25-Compoundierextruder mit Polypropylen als thermoplastisch verarbeitbarem Polymermaterial zu einem Kunststoff-Holzfaser-Verbundwerkstoff verarbeitet (WPC, Wood-Plastic-Composite). Prüfkörper werden aus dem Kunststoff-Holzfaser- Verbundwerkstoff zur Untersuchung der Materialeigenschaften im Spritzgussverfahren gefertigt. Die Oberfläche der Prüfkörper wird gebürstet oder angeschliffen, um die Holzfasern freizulegen, anschließend werden die Prüfungen unmittelbar eingeleitet. The batch is then dried in a circulating air drying oven at 90 ° C. for 16 h (hours). The wood fibers pretreated with the aqueous dispersion are then processed on a ZSK 25 compounding extruder with polypropylene as thermoplastically processable polymer material to form a plastic-wood fiber composite material (WPC, wood-plastic composite). Test specimens are made of the plastic-wood fiber composite material to investigate the material properties by injection molding. The surface of the specimens is brushed or sanded to expose the wood fibers, then the tests are initiated immediately.

Der so erhaltene Verbundwerkstoff besteht zu 60 Gew.-% aus Naturfasern, 31 Gew.-% Polypropylen, 1 ,5 Gew.-% Pigmenten, 4 Gew.-% Hydrophobierungsmittel, 2 Gew.-% Haftvermittler und 2,5 Gew.-% Additive und Gleitmittel. Prüfergebnisse The resulting composite material consists of 60% by weight of natural fibers, 31% by weight of polypropylene, 1.5% by weight of pigments, 4% by weight of hydrophobing agent, 2% by weight of adhesion promoter and 2.5% by weight. % Additives and lubricants. test results

In der 28-tägigen Wasserlagerung (Anlehnung an DIN EN 317) wurde eine Gewichtszunahme an den Proben von ca. 4 Gew.-% ermittelt. In the 28-day water storage (based on DIN EN 317), an increase in weight of the samples of about 4 wt .-% was determined.

Die farbliche Veränderung nach dem Xeno-Test (4.500 h Weatherometer Ci 5000 nach ISO 4892-2-A) konnte mit bloßem Auge ohne direkten Vergleich zum bewitterten Urmuster nicht mehr wahrgenommen werden. The color change after the Xeno test (4,500 h Weatherometer Ci 5000 according to ISO 4892-2-A) could no longer be perceived by the naked eye without direct comparison to the weathered original pattern.

Die Farbveränderung Delta E war 1 ,4. The color change Delta E was 1, 4.

Die Farbveränderung gemäß Graumaßstab nach DIN EN ISO 105 A02 betrug 4 - 5. The color change according to the gray scale according to DIN EN ISO 105 A02 was 4 - 5.

Wesentlich ist das Verhalten des Verbundwerkstoffes bei einer wiederholten Wasserlagerung und Rücktrocknung bis zur Gewichtskonstanz. Während eine Prüfplatte aus einem Wood-Plastic-Composite (WPC), welche unbehandelte Holzfasern enthält, nach Rücktrocknung der Probe bis zur Gewichtskonstanz und erneuter Lagerung im Wasser stetig mehr Wasser aufnimmt, ist dazu im Vergleich die Wasseraufnahme nach wiederholter Lagerung und Rücktrocknung bis zur Gewichtskonstanz bei einer Prüfplatte aus einem Wood-Plastic-Composite (WPC), welche erfindungsgemäß behandel- te Holzfasern enthält, deutlich reduziert. What is essential is the behavior of the composite in repeated water storage and re-drying to constant weight. While a test plate made of a wood-plastic composite (WPC), which contains untreated wood fibers after re-drying the sample to constant weight and re-storage in water steadily absorbs more water, compared to the water absorption after repeated storage and re-drying to constant weight in a test plate made of a wood-plastic composite (WPC), which contains treated wood fibers according to the invention, significantly reduced.

Die Erfindung wird gemäß beigefügter Figuren näher erläutert. The invention will be explained in more detail according to attached figures.

Hierzu zeigt This shows

Fig.1 einen schematischen Querschnitt durch einen Gegenstand aus dem Verbundwerkstoff ; A schematic cross section through an article of the composite material;

Fig.2 eine Grafik zur Wasseraufnahme einer Prüfplatte aus einem Wood-Plastic- Composite (WPC), welche unbehandelte Holzfasern enthält; 2 is a graph for water absorption of a test plate made of a wood-plastic composite (WPC) containing untreated wood fibers;

Fig. 3 eine Grafik zur Wasseraufnahme einer Prüfplatte aus einem Wood-Plastic- Composite (WPC), welche erfindungsgemäß behandelte Holzfasern enthält. In Fig. 1 ist schematisch ein Querschnitt durch einen Gegenstand 1 aus einem thermoplastisch verarbeitbaren Polymermaterial 2 und Naturfasern 3 dargestellt. Fig. 3 is a graph for water absorption of a test plate made of a wood-plastic composite (WPC), which contains wood fibers treated according to the invention. FIG. 1 schematically shows a cross section through an article 1 made of a thermoplastically processable polymer material 2 and natural fibers 3.

Gegenstandgröße und Naturfasergröße sowie Pigmentteilchengröße sind nicht maßstäb- lieh, sondern zur Verdeutlichung des Prinzips der Erfindung frei gewählt. Item size and natural fiber size and pigment particle size are not to scale, but freely chosen to illustrate the principle of the invention.

Die Naturfasern 3 sind in dem thermoplastisch verarbeitbaren Polymermaterial 2 eingebettet. Die Naturfasern 3 sind durch die Vorbehandlung mit der wässrigen Dispersion mit einem Hydrophobierungsmittel 4 beschichtet, das mit der Faseroberfläche der Naturfasern 3 verbunden ist und dort anhaftet. The natural fibers 3 are embedded in the thermoplastically processable polymer material 2. The natural fibers 3 are coated by the pretreatment with the aqueous dispersion with a hydrophobing agent 4, which is connected to the fiber surface of the natural fibers 3 and adheres there.

In dem Hydrophobierungsmittel 4 sind Pigmentteilchen 5 verteilt, die der Naturfaser 3 Far- be verleihen. In the hydrophobizing agent 4 pigment particles 5 are distributed, which give the natural fiber 3 color.

Pigmentteilchen 5 können auch - dies ist in der Fig. 1 nicht gezeigt - oberflächlich in die Poren der Naturfaser 3 eingedrungen und darin gebunden sein.  Pigment particles 5 can also - this is not shown in FIG. 1 - penetrate superficially into the pores of the natural fiber 3 and be bound therein.

Der Gegenstand 1 aus dem thermoplastisch verarbeitbaren Polymermaterial 2 und den Naturfasern 3, auf denen Hydrophobierungsmittel 4 mit Pigmentteilchen 5 anhaftet, weist eine Oberfläche 6 auf, die strukturiert sein kann, insbesondere durch einen Bürstvorgang eine Bürststrukturierung aufweisen kann. The article 1 of the thermoplastically processable polymer material 2 and the natural fibers 3, on which water repellent 4 adheres with pigment particles 5, has a surface 6, which may be structured, in particular by a brushing process may have a Bürststrukturierung.

Fig. 2 zeigt eine Grafik zur Wasseraufnahme einer Prüf platte aus einem Wood-Plastic- Composite (WPC), welche unbehandelte Holzfasern enthält. Fig. 2 shows a graph for water absorption of a test plate from a wood-plastic composite (WPC) containing untreated wood fibers.

Es ist der Verlauf der Gewichtszunahme nach 28-tägiger Wasserlagerung einer gebürsteten WPC Prüfplatte der Größe 100 mm x 100 mm x 3mm (Millimeter), welche im Spritzgussverfahren hergestellt wurde, gezeigt.  The weight gain profile after 28 days of water immersion of a 100 mm x 100 mm x 3 mm (mm) brushed WPC test plate, which was produced by injection molding, is shown.

Ohne Vorbehandlung der Holzfasern nimmt die Wasseraufnahme nach Rücktrocknung der Probe bis zur Gewichtskonstanz (welche bei 80 °C im Umluftofen durchgeführt wurde) und erneuter Lagerung im Wasser stetig mehr Wasser auf.  Without pretreatment of the wood fibers, the water absorption after re-drying the sample to constant weight (which was carried out at 80 ° C in a convection oven) and re-storage in water steadily more water.

Fig. 3 zeigt eine Grafik zur Wasseraufnahme einer Prüfplatte aus einem Wood-Plastic- Composite (WPC), welche erfindungsgemäß behandelte Holzfasern enthält. Dazu ist der Verlauf der Gewichtszunahme nach 28-tägiger Wasserlagerung einer gebürsteten WPC Prüfplatte der Abmessung 100 mm x 100 mm x 3mm (Millimeter), welche im Spritzgussverfahren hergestellt wurde gezeigt. Fig. 3 shows a graph for water absorption of a test plate made of a wood-plastic composite (WPC) containing wood fibers treated according to the invention. In addition, the course of weight gain after 28 days of water storage of a brushed WPC test plate measuring 100 mm x 100 mm x 3 mm (mm), which was produced by injection molding is shown.

Die Holzfasern wurden mit einem Hydrophobierungsmittel auf Melaminbasis vorbehandelt. Im Vergleich zur unbehandelten Faser ist die Wasseraufnahme nach wiederholter Lagerung und Rücktrocknung bis zur Gewichtskonstanz(welche bei 80 °C im Umluftofen durchgeführt wurde) im Vergleich zur unbehandelten Holzfaser deutlich reduziert.  The wood fibers were pretreated with a melamine based water repellent. Compared to the untreated fiber, the water absorption after repeated storage and re-drying to constant weight (which was carried out at 80 ° C. in a circulating air oven) is significantly reduced compared to untreated wood fiber.

- Patentansprüche - - Claims -

Bezugszeichenliste LIST OF REFERENCE NUMBERS

1 Gegenstand 1 item

2 thermoplastisch verarbeitbares Polymermaterial 3 Naturfaser  2 thermoplastically processable polymer material 3 natural fiber

4 Hydrophobierungsmittel  4 water repellents

5 Pigmentteilchen  5 pigment particles

6 Oberfläche  6 surface

7 Verbundwerkstoff  7 composite material

Claims

Patentansprüche claims 1. Wässrige Dispersion zur Behandlung von Naturfasern (3), insbesondere von Holzfasern, enthaltend 1. Aqueous dispersion for the treatment of natural fibers (3), in particular of wood fibers containing ein in Wasser lösliches oder dispergierbares, auf einer Naturfaser haftendendes Hydrophobierungsmittel,  a water-soluble or dispersible hydrophobing agent adhering to a natural fiber, - eine in Wasser dispergierbare Pigmentzubereitung  - A water-dispersible pigment preparation Wasser.  Water. 2. Wässrige Dispersion nach Anspruch 1 , dadurch gekennzeichnet, dass das Hydrophobierungsmittel (4) ausgewählt ist aus einem Epoxidharz, einem Melaminharz, einem harnstoffbasierenden Harz, einem niedermolekularen Wachs, einem Silikonharz, einem Wasserglas, einem Ethylvinylacrylat und einem Ethylmethacrylat. 2. Aqueous dispersion according to claim 1, characterized in that the hydrophobizing agent (4) is selected from an epoxy resin, a melamine resin, a urea-based resin, a low molecular weight wax, a silicone resin, a water glass, an ethyl vinyl acrylate and an ethyl methacrylate. 3. Wässrige Dispersion nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Pigmentzubereitung ausgewählt ist aus anorganischen und / oder organischen Pigmen- ten, umfassend für anorganische Pigmente Weißpigmente, Schwarzpigmente, Buntpigmente und für organische Pigmente Anthanthronpigmente, Anthrachinonpigmente, etc. bis Triarylcarboniumpigmente. 3. Aqueous dispersion according to claim 1 or 2, characterized in that the pigment preparation is selected from inorganic and / or organic pigments, comprising for inorganic pigments white pigments, black pigments, colored pigments and for organic pigments anthanthrone pigments, anthraquinone pigments, etc. to triaryl carbonium pigments. 4. Verfahren zur Behandlung von Naturfasern, umfassend die Schritte 4. A method of treating natural fibers, comprising the steps - Bereitstellen von Naturfasern (3)  - Providing natural fibers (3) Bereitstellen einer wässrigen Dispersion nach einem der Ansprüche 1 bis 3 Inkontaktbringen der Naturfasern (3) mit der wässrigen Dispersion.  Providing an aqueous dispersion according to any one of claims 1 to 3, contacting the natural fibers (3) with the aqueous dispersion. 5. Verfahren zur Behandlung von Naturfasern (3) nach Anspruch 4, dadurch gekenn- zeichnet, dass die Naturfasern (3) mit der wässrigen Dispersion in einem kontinuierlichen Vorgang oder einem diskontinuierlichen Vorgang in Kontakt gebracht werden. 5. Process for the treatment of natural fibers (3) according to claim 4, characterized in that the natural fibers (3) are brought into contact with the aqueous dispersion in a continuous process or a discontinuous process. 6. Verfahren zur Behandlung von Naturfasern (3) nach Anspruch 4 oder 5, dadurch gekennzeichnet, dass die Naturfasern (3) nach Inkontaktbringen mit der wässrigen Dis- persion bis zu einer vorbestimmten Restfeuchte getrocknet werden. Verfahren zur Behandlung von Naturfasern (3) nach einem der Ansprüche 4 bis 6, umfassend weiterhin einen Trocknungsschritt vor dem Inkontaktbringen der Naturfasern (3) mit der wässrigen Dispersion. 6. Process for the treatment of natural fibers (3) according to claim 4 or 5, characterized in that the natural fibers (3) are dried after contacting with the aqueous dispersion to a predetermined residual moisture. A method of treating natural fibers (3) according to any one of claims 4 to 6, further comprising a drying step prior to contacting the natural fibers (3) with the aqueous dispersion. Verbundwerkstoff (7) aus einem thermoplastisch verarbeitbaren Polymermaterial (2) und Naturfasern (3), dadurch gekennzeichnet, dass die Naturfasern (3) mit einer wässrigen Dispersion nach einem der Ansprüche 1 bis 3 behandelt sind. Composite material (7) made of a thermoplastically processable polymer material (2) and natural fibers (3), characterized in that the natural fibers (3) are treated with an aqueous dispersion according to one of claims 1 to 3. Verbundwerkstoff (7) aus einem thermoplastisch verarbeitbaren Polymermaterial (2) und Naturfasern (3) nach Anspruch 8, dadurch gekennzeichnet, dass die Wasseraufnahme bei einer 28-tägigen Wasserlagerung in Anlehnung an DIN EN 317 eines oberflächengebürsteten oder oberflächengeschliffenen Probekörpers kleiner 4 Gew.-% und / oder die Farbveränderung der Oberfläche eines Probekörpers nach einem Xeno- Test (4500 h Weatherometer Ci5000 nach ISO 4892-2) delta E kleiner 1 ,5 beträgt und / oder die Wasseraufnahme in Anlehnung an DIN EN 317 bei einer auch mehrfachen Wiederholung der 28-tägigen Wasserlagerung nach jeweiliger Rücktrocknung des oberflächengebürsteten oder oberflächengeschliffenen Probekörpers bis zur Gewichtskonstanz um mindestens 40 % gegenüber einem Verbundwerkstoff, dessen Naturfasern nicht behandelt sind, reduziert ist. Composite material (7) made of a thermoplastically processable polymer material (2) and natural fibers (3) according to claim 8, characterized in that the water absorption in a 28-day water storage based on DIN EN 317 a surface-brushed or surface-ground test specimen less than 4 wt .-% and / or the color change of the surface of a test specimen after a xeno test (4500 h Weatherometer Ci5000 according to ISO 4892-2) delta E is less than 1.5, and / or the water absorption is based on DIN EN 317 with a multiple repetition of the 28 -day water storage after each re-drying of the surface-brushed or surface-ground test specimen to constant weight by at least 40% compared to a composite material whose natural fibers are not treated, is reduced. 0. Gegenstand (1) aus dem Verbundwerkstoff (7) nach Anspruch 8 oder 9, insbesondere ein Gegenstand aus einem Kunststoff-Holzfaser-Verbundwerkstoff. 0. article (1) of the composite material (7) according to claim 8 or 9, in particular an article made of a plastic-wood fiber composite material.
PCT/EP2012/003340 2011-08-19 2012-08-04 Aqueous dispersion for treating natural fibers and method for treating natural fibers Ceased WO2013026528A1 (en)

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US20110171404A1 (en) * 2004-04-08 2011-07-14 Roland Baker Fibre Polymer Composite (Fpc) Material
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DE2417243A1 (en) * 1974-04-09 1975-11-06 Becker & Van Huellen Fibreboard bonded with synthetic latex dispersions - as natural resin substitute to reduce cost and simplify handling
US5252103A (en) * 1991-02-05 1993-10-12 Matsui Shikiso Chemical Co, Ltd. Pigmenting of cellulose textiles: treatment with cationic compound and immersion in aqueous pigment dispersion
WO2006092330A1 (en) * 2005-03-04 2006-09-08 Basf Aktiengesellschaft Production of moulded bodies from lignocellulose-based fine particle materials

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