EP1999194A1 - Matiere thermoplastique renforcee par des fibres - Google Patents

Matiere thermoplastique renforcee par des fibres

Info

Publication number
EP1999194A1
EP1999194A1 EP07727015A EP07727015A EP1999194A1 EP 1999194 A1 EP1999194 A1 EP 1999194A1 EP 07727015 A EP07727015 A EP 07727015A EP 07727015 A EP07727015 A EP 07727015A EP 1999194 A1 EP1999194 A1 EP 1999194A1
Authority
EP
European Patent Office
Prior art keywords
fiber
reinforced thermoplastic
fibers
airlaid
thermoplastic
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.)
Withdrawn
Application number
EP07727015A
Other languages
German (de)
English (en)
Inventor
Morten Rise Hansen
Ralf Ehmke
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.)
Concert GmbH
Original Assignee
Concert GmbH
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 Concert GmbH filed Critical Concert GmbH
Publication of EP1999194A1 publication Critical patent/EP1999194A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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

Definitions

  • the invention relates to a fiber-reinforced thermoplastic as well as molded or manufactured from it. Furthermore, the invention relates to the use of airlaid cellulosic fiber material for producing such fiber-reinforced thermoplastics.
  • Fiber-reinforced thermoplastic-based composites are increasingly being used in place of metallic materials in many fields of technology because they promise significant weight reduction, with mechanical parameters that are otherwise comparable in many respects.
  • the composite material includes a fibrous component which has a considerable influence on mechanical properties, in particular tensile and flexural strength as well as impact resistance of the composite material.
  • fibrous components are used (i) fibers of inorganic materials such as glass, carbon and boron, (ii) metallic fibers, e.g. As steel, aluminum and tungsten, (iii) synthetic organic fibers, for.
  • Other auxiliaries and fillers may be added to the composite.
  • glass fiber reinforced thermoplastics in vehicle construction, eg for vehicle interior trim.
  • the production of glass fibers requires the use of significant amounts of energy and the base materials are not of biological origin, so that the sustainability of the manufacturing process is environmentally critical to criticize.
  • the disposal of glass fiber reinforced thermoplastics is difficult, as even with thermal decomposition of the material considerable amounts of residues remain, which can be fed to a landfill usually only.
  • glass fiber has a high abrasiveness, so that the processing of the materials is difficult in the context of conventional processing methods for thermoplastics.
  • DE 103 35 139 A1 discloses a method for producing a component from a fiber composite material, in which 3-10 mm long artificial cellulose regenerated fibers are mixed with a thermoplastic as the fiber-reinforcing component. The resulting material is used as a base material for the production of lightweight components.
  • WO 97/30838 A1 describes a fiber composite material of natural cellulose fiber material, here wood flour and a thermoplastic. The material is extruded directly to the component.
  • natural fiber materials as a fiber-reinforcing component is offset by inferior mechanical properties of the resulting composite materials as compared to fiber-reinforced composites with glass fiber content.
  • natural fibers such as flax, hemp or even wood particles of varying composition: Depending on the growing area, cultivation period, storage and possibly pretreatment, individual batches of the material differ. However, this also varies the mechanical characteristics of the fiber-reinforced thermoplastics to be produced, which makes the technical use difficult. The material can continue to change its shape and appearance due to progressive degradation processes. Finally, the natural sulfur and nitrogen content in natural products can lead to the outgassing of undesirable odors.
  • WO 03/104309 A1 describes a fiber composite material to which cellulosic fibers are added from pulp, wherein the cellulose used is an ⁇ -cellulose with a degree of purity of> 80%.
  • the polymeric matrix is a polymer having a melting point of ⁇ 200 ° C, z. B. a polypropylene.
  • the composite further contains at least one water-soluble binder, at least one lubricant and at least one adhesion promoter.
  • the use of cellulose fibers has the advantage that the stiffness and impact resistance of the resulting composite material is increased, there is a global availability of cellulose fibers and the consistency of the starting materials and the composite material is increased.
  • the object of the present invention is to utilize the advantages associated with the use of organic materials of natural origin, while further improving the processing and use-relevant properties of the composite material.
  • thermoplastic comprising:
  • thermoplastic matrix b
  • the spreading material accordingly contains, as a fiber-reinforcing component, a cellulose fiber material in the form of an airlaid. It has been found that the use of this fiber material leads to an increase in the impact resistance and impact strength as well as tensile and flexural strength compared to the use of cellulose fibers not subjected to this processing process, from fibrous cellulose, but also to wood-discarded thermoplastics. The reason for this behavior is not fully understood yet. It is believed that nonwoven production results in a fiber bond between individual cellulosic fibers, which is at least partially retained even in the subsequent comminution or processing of the web.
  • An airlaid cellulose fiber material in the context of this invention is a material containing cellulose fibers, in particular made from fiber pulp by the sulphate or sulphite process and fragments of a corresponding airlaid nonwoven.
  • the airlaid nonwoven fiber pulp is separated mechanically with the aid of hammer mills.
  • the fibers are randomly deposited over a stream of air onto a belt to form a sheet-like body (air laid web forming).
  • Subsequent binding of the fibers can be achieved by bonding with aqueous dispersions (eg polyacrylates, polyvinyl acetates, ethylene vinyl acetates, styrene butadiene and other latexes), by heat treatment of binder fibers or treatment with ultrasound or high frequency.
  • aqueous dispersions eg polyacrylates, polyvinyl acetates, ethylene vinyl acetates, styrene butadiene and other latexes
  • the fleece density can be adjusted by controlled roller pressure and temperature. Details of the airlaid process can be found inter alia in the patents US 4,494,278, US 5,527,171 and US 4,640,810. the content of which is hereby incorporated by reference for purposes of disclosure
  • a fiber-reinforcing component it is particularly preferred to use a spreading material which is obtained by comminution of a fleece made of lignin-free fiber pulp produced by the airlaid process.
  • Shredding in the sense of the invention involves the mechanical dismemberment of the nonwovens.
  • the processed airlaid nonwovens preferably have an average length-weighted fiber length in the range of 0.5 to 5 mm, more preferably 2 to 3 mm, prior to comminution.
  • the length-weighted fiber length is calculated as the quotient of the sum of all fibers multiplied by the corresponding squares of the length by the sum of all fibers multiplied by the corresponding lengths (measurement method: ISO 16065-1 standard 2001-09) Fiber materials - Determination of the fiber length by automatic optical analysis - Part 1: Method with polarized light).
  • This fiber length specification refers to the average length of the cellulosic fibers, not the length of the shredded airlaid cellulosic fiber material. This length is no longer clearly determinable after passing through agglomeration, but certainly greater than that of the cellulose fibers.
  • thermoplastic according to the invention it is conceivable not only to collect a comminuted airlaid nonwoven itself, but also preferably residual waste from the industrial production and processing of airlaid nonwoven, to comminute it and to use it in the sense according to the invention.
  • Remnants of nonwoven production after the airlaid process or in the further processing stages of the material are so far nert, pressed and dumped or burned.
  • the combustion of the material requires a quality control of the combustion process, so that it can only be carried out in special plants.
  • absorbent hygiene products include, in particular, feminine and diaper hygiene products.
  • Fiber pulp which is particularly preferred as the major constituent of the cellulosic fiber material, is a specialty product of industrial pulp production and can be obtained via both the acid sulfite and the alkaline sulfate (Kraft) processes.
  • the lignin content is lowered from previously typically 30% to 10%.
  • the hemicellulose content is also attacked, but is about 12% greater in the widely used sulphate process after treatment over the sulphite process.
  • delignifying bleaching steps to increase the degree of whitening with oxygen (oxygen delignification), hydrogen peroxide brighteners (peroxide brightening) and ozone bleaching. Used for bleaching chlorine-oxygen compounds are hardly used.
  • the delignified fiber pulp is converted into a transportable form by a wet paper-laying process, dewatering, drying and rolling or cutting of plates.
  • This flaky, easily shredded fiber pulp (Fluff PuIp) can be processed well in the airlaid process.
  • Fiber pulp is the name given to the fine, predominantly cellulose pulp resulting from the pulping of wood or other plant fibers Dimensions. It is a refined natural product, is present as a white, fibrous solid at room temperature and has a cellulose content of over 95 wt.%.
  • Fiber pulp is largely free of lignin, with lignin-free in the context of the invention referring to a lignin content of ⁇ 0.5% by weight of the total weight of the (dry) fiber pulp.
  • Lignin can be determined as a hydrolysis residue taking into account the residue of ignition by acid hydrolysis of the cellulosic constituents.
  • NIR near-infrared
  • the residual lignin content determined in accordance with DIN 54356 and as a visible property by specifying the spectral reflection factor brightness according to ISO 2469 / ISO 2470, usually over 75%, better over 85%.
  • the properties of the fiber pulp depend both on the type of wood used, as well as on the manufacturing process used and are subject to fluctuations.
  • airlaid cellulosic fiber material with longer-fiber softwood softwood fiber pulp is used as a fiber-reinforcing component of the thermoplastics because it is based on e.g. Pine-made fibers have a higher tensile strength.
  • the hemicellulose content in the case of fiber pulp is about 12%, based on the total weight of the (dry) fiber pulp.
  • Chemical pulp is used in the food, cosmetics and pharmaceutical industries and in the production of synthetic fibers from regenerated cellulose such as viscose, cellulose acetate, lyocell, cellulose carbamate u.a.
  • Cellulose is the isotactic beta-1,4-polyacetal of cellobiose and forms unbranched, water-insoluble chains.
  • the average molar masses are 50,000 - 500,000.
  • alpha-cellulose is called the at 20 ° C in 17.5% iger NaOH or 24% KOH insoluble fraction with an average degree of polymerization>200; the fraction which precipitates from the sodium-alkaline solution with methanol becomes beta-cellulose and the non-precipitable fraction gamma-cellulose, the latter both together also called hemicellulose.
  • the cellulosic fibers are based on the so-called elementary fibril, which is visible with the electron microscope. Several elementary fibrils form microfibrils and macrofibrils.
  • Thermoplastic is the name given to polymeric materials which are soft or hard at service temperature and which have a flow transition region above the service temperature.
  • Thermoplastics consist of linear or branched polymers, which in the case of amorphous thermoplastics above the glass transition temperature (T g ), in the case of (partially) crystalline thermoplastics above the melting temperature (T m ) are in principle fluid. They can be processed in the softened state by molding, extrusion, injection molding or other molding processes to form parts.
  • Important thermoplastics are polyethylenes, polypropylene, polystyrene, polyvinyl chloride, polyacrylonitrile, polyamides, polyesters and polyacrylates. It is also possible to use blends of various thermoplastic polymers as the polymeric matrix.
  • the thermoplastic need not be a homopolymer, but may also be present as a copolymer, polypolymer, block polymer, or otherwise modified polymer.
  • the thermoplastic matrix is a polypropylene or contains a polypropylene as a main component in a blend, ie polypropylene has a weight fraction of ⁇ 50% of the thermoplastic matrix.
  • Composite materials on this polymeric basis are easy to process - also in granular form or as a semi-finished product - and show favorable mechanical characteristics, in particular for use in vehicle construction, eg. B. for interior trim.
  • to increase the tensile or flexural strength - in each case with the focus on the desired application to increase the adhesion between the polymeric matrix and the fiber-reinforcing component.
  • a polypropylene modified to enhance an interaction with cellulose in particular polypropylene-maleic anhydride graft copolymer (MAPP).
  • MAPP polypropylene-maleic anhydride graft copolymer
  • the modified polypropylene or other adhesion-enhancing component is added to the polymeric matrix or / and the fiber-reinforcing component.
  • the airlaid cellulosic fibrous material comprises a binder for maintaining a bond between fibers of the airlaid cellulosic fiber material selected from the group consisting of (i) a fibrous or granulated thermoplastic, preferably polyethylene and / or polypropylene and / or polyethylene terephthalate, (ii) thermoplastic encapsulated fibers, (iii) a latex, preferably a self-crosslinking or crosslinked EVA latex, a vinyl emulsion including vinyl acetate or other vinyl ester based emulsions in the form of homopolymers or copolymers with ethylene and ethylene or acrylic monomers, acrylic emulsions in the form of homopolymers or copolymers, or other crosslinked adhesives, and mixtures of two or more of these binders according to (i) to (iii).
  • a binder for maintaining a bond between fibers of the airlaid cellulosic fiber material selected from the group consisting of
  • the so-called two-component fibers which have a core of polypropylene or of polyethylene terephthalate, and a sheathing of polyethylene are to be emphasized as binders.
  • the polyethylene of the sheath acts as the actual binder between the bicomponent or bicomponent fibers, which retain their fibrous structure when melting the polyethylene due to their higher melting core and are thus suitable to keep the cellulose fibers.
  • suitable binders are polyester-copolyester core-sheath fibers and multicomponent fibers.
  • Polyester-copolyester core-sheath fibers are particularly suitable since low-melting copolyesters with similar temperature windows as polyethylene are also available.
  • the binders usually allow that binding between the fibers of the cellulose fiber material is maintained even when liquid contact.
  • the binders further promote the reinforcing effect of the airlaid cellulosic fibrous material in the fiber reinforced thermoplastic by improving the bulk of the fibrous material during processing and in the final thermoplastic. This is particularly advantageous when using a spreading material made of airlaid cellulose fiber material.
  • thermoplastics which contain superabsorbent polymers (SAP).
  • SAPs superabsorbent polymers
  • SAPs are polymeric gelling compounds that are capable of binding very large amounts of water without deliquescing, such as the water-insoluble starch produced by alkaline hydrolysis of starch / acrylonitrile copolymers.
  • Acrylamide / acrylic acid graft copolymers or also crosslinked polyacrylic acids After processing the granules into shaped parts, a reduction of the outgassing can be achieved.
  • auxiliaries and additives may be present in the thermoplastic according to the invention.
  • Auxiliaries may be, in particular, fillers, stabilizers, antistatic agents, flame retardants, masterbatch colorants in the form of 1-3% based on total granules, flexibilizers and plasticizers, adhesion promoters, blowing agents, antibacterial agents and fungicides.
  • Suitable fillers are inorganic materials such as chalk, limestone, marble, aluminum, quartz, metal, mica, etc.
  • thermoplastic preferably has the following composition:
  • thermoplastic matrix 30 - 90 parts by weight of thermoplastic matrix
  • thermoplastic of said composition can be easily processed, be it granules, semi-finished or otherwise suitable for processing.
  • the components are mixed together in a conventional manner and optionally pieced.
  • the thermoplastic contained by thermal or physico-thermal agglomeration of the components is preferably provided as granules or semi-finished products for further processing.
  • the resulting thermoplastic is storable granules, logistically easy to handle and easy to use in further processing.
  • Cellulose fibers made of fiber pulp are white, so that the addition of colorants compared to natural fibers is significantly expanded.
  • thermoplastic in vehicle construction, in particular for the production of components of3.1innenraumverklei- Phys, such as side door covers, front area, parcel shelf and vehicle roof.
  • components of3.1innenraumverklei- Phyg such as side door covers, front area, parcel shelf and vehicle roof.
  • the fiber-reinforced thermoplastic or granules or semi-finished product based on the thermoplastic is for the manufacture of housings and packaging materials, e.g. of containers, especially in vehicle construction, particularly suitable.
  • thermoplastic according to the invention is advantageously suitable for forming a molded part, in particular for use in the automotive industry. Particularly advantageous in such a molded part is the high impact strength and notched impact strength achievable by using a thermoplastic according to the invention while at the same time saving material of the cost-intensive thermoplastic matrix.
  • Example 1 Remnants of airlaid nonwoven production / processing
  • the grit obtained typically has the following composition:
  • the core is predominantly polypropylene or polyethylene terephthalate and the shell is a polyethylene-derived polymer.
  • the fiber length is 3 - 18 mm.
  • a superabsorbent polymer namely a polyacrylate.
  • SAP superabsorbent polymer
  • modified starch or other water-insoluble gel-forming polysaccharides can be used.
  • Remnants from the manufacture and processing of diapers are shredded in a shredder.
  • the grit obtained has the following typical composition:
  • Nonwovens come from.
  • the fiber length is 2 - 3 mm.
  • a superabsorbent polymer namely a polyacrylate.
  • SAP superabsorbent polymer
  • modified starch or other water-insoluble gel-forming polysaccharides can be used.
  • the core is predominantly made of polypropylene or polyethylene terephthalate, and in the case of two-component fibers, the shell of a polyethylene-derived polymer.
  • the fiber length is 3 - 18 mm.
  • the remnant is mixed in a weight ratio of 1: 1 with pellets of pure polypropylene and agglomerated by thermomechanical processing. Pelleting the product provides a granule.
  • thermoplastics according to the invention Comparison of impact strength and notched impact strength of thermoplastics according to the invention with other materials
  • Polypropylene granules (hereafter "PP”, Borealis HK 060 AE) were mixed with wood flour (hereinafter “wood”) or airlaid cellulose fiber material (“cell”) mixed and injection-molded into 4 mm thick ISO standard bars in the ratios given in Table 1:
  • the mold temperature was 25 ° C, o.
  • the airlaid cellulosic fiber material contained 70% by weight fluff pulp cellulose, 10% by weight synthetic fibers of polyethylene, polypropylene and / or polyethylene terephthalate, 8% by weight latex, 10% by weight superabsorbent polymer particles, balance polypropylene carrier ,
  • the ISO standard bars produced were reinforced in accordance with DIN EN ISO 179/1 eAU with a pendulum percussion hammer at 23 ° C. (impact resistance pendulum without notch: 5 J unreinforced [100% PP], 2 J [remainder]; impact value pendulum with notch: 0.5 J) for impact resistance and notched impact strength. Table 2 shows the results:
  • thermoplastics according to the invention Comparison of the outgassing values of thermoplastics according to the invention with other materials
  • the fiber-reinforced thermoplastics according to the invention in some cases significantly better, in comparison with wood-reinforced thermoplastics and pure polypropylene, in particular from a proportion of 25 wt .-% of airlaid cellulose fiber material. lower, have condensate values and so a significant requirement of the automotive industry for reduced condensation of volatiles to discs o.a. progeny.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Reinforced Plastic Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

L'invention concerne une matière thermoplastique renforcée par des fibres contenant un matériau à base de fibre de cellulose air-laid, ainsi que ses utilisations.
EP07727015A 2006-03-22 2007-03-16 Matiere thermoplastique renforcee par des fibres Withdrawn EP1999194A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006013988A DE102006013988A1 (de) 2006-03-22 2006-03-22 Faserverstärkter Thermoplast
PCT/EP2007/052536 WO2007107527A1 (fr) 2006-03-22 2007-03-16 Matiere thermoplastique renforcee par des fibres

Publications (1)

Publication Number Publication Date
EP1999194A1 true EP1999194A1 (fr) 2008-12-10

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EP07727015A Withdrawn EP1999194A1 (fr) 2006-03-22 2007-03-16 Matiere thermoplastique renforcee par des fibres

Country Status (7)

Country Link
US (1) US8530548B2 (fr)
EP (1) EP1999194A1 (fr)
JP (1) JP2009530462A (fr)
CN (1) CN101405328B (fr)
CA (1) CA2645113A1 (fr)
DE (1) DE102006013988A1 (fr)
WO (1) WO2007107527A1 (fr)

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CN101405328B (zh) 2013-07-03
JP2009530462A (ja) 2009-08-27
CN101405328A (zh) 2009-04-08
US8530548B2 (en) 2013-09-10
US20090306253A1 (en) 2009-12-10
CA2645113A1 (fr) 2007-09-27
DE102006013988A1 (de) 2007-09-27

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