WO2007101896A1 - Matériau composé, procédé de production et utilisation de celui-ci - Google Patents
Matériau composé, procédé de production et utilisation de celui-ci Download PDFInfo
- Publication number
- WO2007101896A1 WO2007101896A1 PCT/ES2007/000117 ES2007000117W WO2007101896A1 WO 2007101896 A1 WO2007101896 A1 WO 2007101896A1 ES 2007000117 W ES2007000117 W ES 2007000117W WO 2007101896 A1 WO2007101896 A1 WO 2007101896A1
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- WO
- WIPO (PCT)
- Prior art keywords
- composite material
- fibers
- spindle
- stage
- minimum
- Prior art date
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- PCVVBHUFWPHCAL-UHFFFAOYSA-N butane-1,4-diol;terephthalic acid Chemical compound OCCCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 PCVVBHUFWPHCAL-UHFFFAOYSA-N 0.000 claims description 5
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- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/28—Moulding or pressing characterised by using extrusion presses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
- B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
- B29B7/482—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws provided with screw parts in addition to other mixing parts, e.g. paddles, gears, discs
- B29B7/483—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws provided with screw parts in addition to other mixing parts, e.g. paddles, gears, discs the other mixing parts being discs perpendicular to the screw axis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
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Definitions
- This invention relates to composite materials comprising cellulosic materials that serve even for moderately demanding applications, such as those in the sectors of manufacture of electrical, electronic and telecommunications material, and can thus replace different thermosetting polymers and fiber reinforced materials. of glass, currently used. Additionally, the present invention relates to a method for the continuous production of said composite materials to which it refers and to the use of said composite materials for the manufacture of various moldable articles.
- Thermosetting polymeric materials are not recyclable. In addition, the cycle times for injection molding are long. In the case of laminar molding compounds such as those used in compression molding of thermosetting prepregs (SMCs), a lot of labor is required and the production process is relatively rudimentary and difficult to automate. Therefore, production costs are high.
- Thermoplastic materials are relatively expensive, difficult to recycle and, their waste, difficult to treat, due to their content of glass fibers, which are not biodegradable.
- its density is relatively high (around 2.5-2.8 kg / m 3 ), resulting in molded articles that are heavier than desirable.
- the abrasion produced by glass fibers in processing equipment is notable, resulting in higher production costs because the change of the various parts of the processing equipment has to be carried out more frequently (eg, the spindles of injection molding machines).
- cellulosic materials such as fillers and reinforcements in polymer matrix composite materials.
- Cellulosic materials are composed of different types of particulate fillers and reinforcements derived from a multitude of plant species and tree or wood species, whose main components are cellulose, hemicellulose and lignin, among others.
- Cellulosic materials have some important advantages over inorganic materials such as talc, mica or glass fibers, traditionally used as fillers and reinforcements in polymer matrix composite materials. Mainly, these advantages are: lower density, lower cost, less abrasion of processing equipment, biodegradability and renewable character.
- cellulosic materials have several disadvantages:
- the developed composite materials can be divided into two groups: 1) Composite materials whose main component is a cellulosic material. 2) Composite materials whose main component is a polymer. Depending on the type of cellulosic materials and polymers used, their relative proportion in the composite material and the formulation of the composite material as a whole, the methods of obtaining the composite materials and their potential applications can vary widely.
- the prior art includes various formulations of composite materials based on cellulosic materials from a multitude of potential sources of raw materials (cellulosic, virgin or residual fibers, from plant or herbaceous plants, or tree or wood species).
- raw materials cellulosic, virgin or residual fibers, from plant or herbaceous plants, or tree or wood species.
- the most relevant attempts of the prior art state for Solving the problems encountered in trying to combine different types of polymers and cellulosic materials, include different approaches.
- patent application WO9605347 in the name of SKILLICORN describes a series of formulations of composite materials composed of cellulose fibers of different plant plants (among others, jute or kenaf) and a thermoplastic selected from the group of polypropylenes or polyethylenes.
- This invention provides a multitude of applications for these formulations of composite materials: packaging, small appliances, furniture, building materials, automotive products, among many others.
- the composite materials disclosed by it can be transformed by injection molding, compression molding, extrusion, rotational molding or blow molding.
- different techniques can be used to mix between 20 to 60%, by weight, of cellulose fibers coated with a malleable polypropylene, with 80 to 40%, by weight, of polypropylene.
- These techniques include cold compression and pelletizing devices, the Banbury mixer, the Farrell continuous mixer or the single-screw and twin-screw extruders.
- One of the objectives of the method used to obtain the composite material is to maximize the slenderness -relation length / diameter- of the fibers. With this objective and in order to maintain an adequate dispersion of the fibers in the composite material, the use of less intensive mixers such as continuous kneaders or appropriately configured double screw extruders is recommended.
- the EP0426619 patent to ICMA SAN GIORGIO describes a method for the continuous production of mouldable panels obtained from a polymer with high melting temperature (T your ng> 150 ° C) and a thermosensitive filler by direct extrusion using a corroding double screw extruder.
- the method corresponding to the invention comprises the use of three or, preferably, four helical extrusion sections for transport or effective feeding, and two or, preferably, three interposed kneading sections.
- the cylinder or chamber of the extruder used in said invention has three openings or ports. The first opening serves to feed the polymer. The second opening serves to feed the heat-sensitive filling and the third opening for venting or degassing.
- the spindles of the extruder of the invention consist of helical extrusion sections, which have a typical angle, shape and depth of channel, but not considered critical.
- the distance between the cylindrical spaces defined by the rotation of the spindles of the extruder and the integral mixing and extrusion space varies between 0.2 and 2 mm.
- EP0611250 in the name of ICMA SAN GIORGIO describes a method for the extrusion of composite materials based on low melting temperature polymers (T fUs ón ⁇ 150 ° C) for the continuous production of typical semi-finished products, such as PVC panels
- T fUs ón ⁇ 150 ° C low melting temperature polymers
- thermoplastic polymers that can be used to make composite materials comprise so-called general-purpose plastics, such as polyolefins and polystyrene, or engineering plastics. In addition to virgin thermoplastics, recycled thermoplastics can also be used instead.
- a coupling agent to the polymeric material.
- the preferred ratio of polymer to coupling agent for a polyolefin matrix is 70 to 6, with the most preferred ratio being 8 to 16, by weight.
- Preferred coupling agents for such matrices are polyethylenes grafted with maleic anhydride or polypropylenes grafted with maleic anhydride, depending on the type of matrix used.
- Other additives, such as pigments, antioxidants, flame retardants and fillers such as talc, calcium carbonate and carbon black, can also be added to the polymer.
- the pellet of composite material obtained following the process indicated in the patent is considered suitable for obtaining articles by injection molding and compression molding.
- the process revealed by the patent is advantageous because the individual or elementary fibers retain their high slenderness and length.
- the location of the zones of the extruder is calculated from the head of the same, because it is important that the fiber feeding port is located as close as possible to the end of the extruder. Therefore, cellulose fibers are introduced into the melt as late as possible, so that they are minimally affected by friction and heat.
- the extruder claimed by the invention comprises all extruders with two separate feed ports and a degassing port.
- the extruder claimed is divided, according to the authors of the invention, into four zones: a first zone where the polymer is fed, a second zone where the cellulose fibers are fed, a third zone for venting or degassing and a fourth zone in where the pressure is increased.
- Patent application US 5288772 in the name of Clemson University provides a thermoplastic formulation reinforced with cellulose fibers that allows the production of composite materials.
- Another object of said patent is to provide a method to use residual cellulosic and thermoplastic materials.
- the thermoplastic resin present in the composite material can be any thermoplastic (polyolefins, vinyl polymers, polyamides, acrylic resins and styrene resins).
- the cellulosic materials included in said invention can be any material containing cellulose fibers (newspapers, cardboard, wood fibers, scratches, cottons, ramie, jute, bagasse, among many others).
- lignin can be added to the formulation, as well as independent component, or already forming part of the cellulosic materials themselves.
- Another object of the patent is to provide a method for obtaining said composite materials. According to said method, thermoplastic resins are heated in a mixing device until a molten matrix is obtained. Then, while stirring the molten matrix of thermoplastics is continued, the cellulosic materials are added thereto, maintaining the selected temperature.
- US5516472 in the name of STRANDEX describes a composite material comprising a polymer and cellulosic fibers, as well as the process and the machine for manufacturing said product.
- the composite material is characterized by having a high content of cellulose fibers (more than 50%, by weight). According to the authors of the patent, using the continuous low temperature extrusion process revealed by the patent, the material could have up to a 1: 0 fiber / thermoplastic ratio.
- EP799679 in the name of AIN ENGINEERING KK refers to a method for achieving a drawing, such as a wood grain with the appearance of natural wood, on the surface of a synthetic board.
- Said board is constituted by a mixture containing between 20-65%, by weight, of a wood flour, and 35-80%, by weight, of a thermoplastic. If the thermoplastic used is polypropylene or polyethylene, the preferred content of wood flour varies between 50-55%, by weight.
- the synthetic board is manufactured by extrusion, using a single or multi-spindle extruder.
- Patent application US2003 / 00301176 in the name of THERMO FIBERGEN presents as a novelty that high levels of sludge from papermaking can be mixed (eg, up to 70-75%), transformed into granules by wet way, with plastic and , if desired, cellulose fiber, to obtain composite materials.
- the authors of the invention indicate that, surprisingly, despite the low relative levels of plastic, composite materials have good mechanical properties (high strength, high modulus, high impact resistance, among others). These mechanical properties make the composite materials object of the patent useful as raw material for the manufacture of different products, such as roof tiles, fences, door panels, acoustic screens, roofing materials, decorative wall coverings and similar applications. However, the examples show that the mechanical properties of composite materials are poor.
- the sludge from the manufacture of cellulose, lignin, hemicellulose, calcium carbonate, clay and other inorganic components paper In many cases, the ashes of the sludge from papermaking total up to 50% (and in some cases, up to 80% or more) of the volume of sludge.
- the main components of the ashes are calcium carbonate (20-75% of the dry mud) and clay. These two minerals are commonly used in paper as a coating and a filler to improve its mechanical characteristics as well as its appearance.
- the granules obtained by wet transformation of the sludge of papermaking, used as raw material, in combination with rice husk, to obtain the composite materials object of the patent are composed of: Paper fiber (CAS # 9004-34- 6): 47-53%; Kaolin: 28-34% (CAS # 1332-58-7); Calcium carbonate (CAS # 471-34-1): 14-20%. Titanium dioxide (CAS # 13463-67-7): ⁇ 1%.
- the composite material can also contain, together with the granulated sludge of papermaking, different types of cellulose fibers from different sources: short fibers of agricultural origin; fibrous plant materials; fibers from the processes of textile fiber production and processing operations of cellulose pulp and paper; fibers from the recycling processes of paper and wood products, etc.
- the organic material of the composite material comprises the granulated sludge, alone or in combination with cellulose fibers.
- the claimed composite material is manufactured by mixing certain amounts of its components to give rise to a homogeneous mixture, which is then fed to a twin screw extruder.
- the method followed to manufacture the composite material involves the prior obtaining of a homogeneous mixture of the components of the composite material, instead of its direct separate feeding to the extruder, which represents a further stage in the process of obtaining and Higher production cost.
- the resulting composite material is pelleted and fed to a single screw extruder to shape the final product.
- the invention provides, on the one hand, new and effective composite materials, and on the other hand, a new use for the pulp and paper sludge.
- Patent application WO01 / 83195 in the name of DAVIS STANDARD CORP, MURDOCK DAVID E., SNEAD DALE K, DARDENNE DARRELL S. and MILLS IAN W. describes an extrusion process for the manufacture of plastic matrix composites containing particles of wood or wood fibers, whose humidity can be variable and / or high.
- the wood fibers can come from soft wood species -conifers- and / or hardwood species -frondosas-, being the most popular for obtaining profiles, pine, maple and oak.
- organic fillers such as grass residues, agricultural residues, natural fibers from land or aquatic plants, can also be used.
- the process revealed by this patent uses a double screw spindle extruder to dry the organic filling, as well as at least a second extruder to melt the polymer and feed it into the cylinder of the first extruder.
- the process corresponding to the invention uses spindle rotation speeds and shear speeds, lower than traditional equipment and processes.
- the state of the existing technique describes various formulations of composite materials that are suitable for a multitude of applications.
- none of these formulations of composite materials meets the requirements set to the raw materials currently used for some moderately demanding applications, such as those in the sectors of manufacturing of electrical, electronic and telecommunications equipment, or others such as The construction, aviation, automotive, furniture and packaging.
- cellulosic fibers of tree or wood species are different from cellulosic fibers from plant plants.
- Cellulosic fibers from soft wood tree species - whose lengths are between 0.7-1.6 mm approximately - differ from those that come from hardwood tree species - whose lengths are between 2.7-4, 6 mm, approximately.
- the cellulosic fibers of plant plants - whose lengths are between 0.7-250 mm approximately - differ from each other.
- residual cellulosic fibers differ from virgin cellulose fibers.
- the cellulosic fibers obtained by different insulation processes e.g., the different mechanical, chemical and chemical thermomechanical processes for obtaining cellulose pulp
- bleaching processes and refining processes have different characteristics.
- the type of treatments to which the cellulosic fibers can be subjected to be obtained in the desired final form also affects their quality.
- all these factors mentioned condition the morphology of the individual fibers and the characteristics of the agglomerates that they can form (that is, their morphology and apparent density).
- all these factors condition the possibilities of continuously feeding and dosing cellulosic fibers to mixing equipment with molten polymers that can allow the obtaining of composite materials, as well as the properties of the composite materials themselves.
- the prior art does not take into account that the means necessary for dosing the longer cellulose fibers, which are presented in the form of skeins or strands, are different from the means necessary for dosing shorter cellulose fibers.
- thermoplastic matrix composite materials comprising cellulosic materials. These new materials make it possible to replace thermosetting polymers and glass fiber reinforced materials, currently used in various sectors, such as the manufacturing of electrical, electronic and telecommunications equipment. It is also the object of the present invention to provide a new method for the continuous production of said composite materials, as well as some of the molded products that can be manufactured using said composite materials as raw material. Thus, the technology described in this application allows obtaining, in a technical and economically viable way, new thermoplastic matrix composite materials comprising cellulosic materials.
- Figure 1 is a side view of an installation used in the method according to the present invention for obtaining the composite material.
- Figure 2 represents a side view of the corroding extruder with an illustration of the types of spindle elements that can be inserted on each of the mandrels thereof to give rise to different spindle configurations.
- Figure 3 shows a fuse holder base for blade fuses made of the composite materials object of this invention.
- Figure 4 shows a fuse holder base for cylindrical fuses made of the composite materials object of this invention.
- Figure 5 shows the body of the closed vertical tripolar bases manufactured with the composite materials object of this invention. DESCRIPTION OF THE INVENTION
- the present invention refers to a composite material that, for every 100 parts of its weight, comprises: (A) between 25 and 90 parts, by weight, of a thermoplastic polymer; (B) between 1 and 50 parts, by weight, of a cellulosic material, (C) between 0.1 and 15 parts, by weight, of a coupling agent; (D) between 0.05 and 3 parts, by weight, of a primary antioxidant; (E) between 0.05 and 6 parts, by weight, of a secondary antioxidant (F) between 1 and 40 parts, by weight, of a flame retardant, characterized in that said cellulosic material (B) comprises fibers that are selected from the group formed by virgin cellulose pulp fibers from hardwood tree species, fibers obtained as waste from the pulp and paper industry, fibers obtained as waste from the synthetic and textile fiber manufacturing industries, fibers from solid urban and industrial waste or mixtures thereof.
- said thermoplastic polymer (A) is a polyolefin, which is selected from the group consisting of polypropylene homopolymers, propylene copolymers, polypropylene-polyethylene vinyl acetate (PP) + EVA), high density polyethylene, low density polyethylene), a polystyrene (which is selected from the group of its homopolymers, copolymers or terpolymers), polyvinylchloride (PVC), a polymer from the polyamide group, poly (ethylene glycol terephthalate) (PETP), poly (butylene glycol terephthalate) (PBTP), poly (methyl methacrylate) (PMMA) or polycarbonate (PC) or mixtures thereof.
- PETP poly (ethylene glycol terephthalate)
- PBTP poly (butylene glycol terephthalate)
- PMMA poly (methyl methacrylate)
- PC polycarbonate
- the preferred virgin polyolefins for carrying out this invention are polypropylene homopolymers and copolymers of controlled rheology with similar melting points and flow rates ranging from 12 to 150 g / 10 minutes (according to ISO 1133, at 230 0 C and 2 , 16 kg).
- thermoplastic polymers come from industrial waste from the transformation of plastics (eg, any polypropylene, polyethylene, polystyrene or polypropylene co-polyethylene-vinyl- acetate (PP + EVA)) or of the comment of urban solid waste.
- plastics eg, any polypropylene, polyethylene, polystyrene or polypropylene co-polyethylene-vinyl- acetate (PP + EVA)
- PP + EVA polypropylene co-polyethylene-vinyl- acetate
- the recommended coupling agents (C), in accordance with the present invention, are those belonging to the group of polyolefins grafted with maleic anhydride, said polyolefins having number average molecular weights between 2000 and 50,000 or mass average molecular weights comprised between 4000 and 300000, and having maleic anhydride contents comprised between 0.1 and 20%, by weight; pure or modified polyethyleneimines whose molecular weights vary between 800 g / mol-g and 200000 g / mol-g, which are presented as anhydrous products or not; aromatic and aliphatic organosilanes or mixtures thereof.
- the composite material according to the present invention comprises cellulose fibers from hardwood tree species, such as Eucalyptus globul ⁇ s.
- Said cellulose fibers may be virgin cellulose pulp fibers, either raw, bleached or refined.
- the virgin raw cellulose pulp fibers have the following approximate composition (on a dry basis): 97%, by weight, holocellulose, 2.5%, by weight, lignin and 0.5%, by weight, ash.
- Virgin bleached or refined cellulose pulp fibers contain cellulose, for the most part, and very small proportions of lignin and hemicelluloses.
- said fibers obtained as residues of the pulp and paper pulp industry can be residual pulp pulp fibers of the pulp pulp production processes from wood species, from the rejections of the sieving processes of the mixture of cellulose fibers and black liquor leaving the digesters, of the final rejections of the purification processes of the cellulose pulp, and of various losses and leaks through the fabrics of the scrubbers used in the different phases of the bleaching of the cellulose pulp and through the sheet-forming fabric in the window dressing machine.
- Said residual cellulose pulp fibers, after being subjected to filtration and compaction are presented in the form of agglomerates with a humidity comprised between 50-70%, by weight, and which may also contain "uncooked".
- Said agglomerates have the following approximate composition (on a dry basis): between a 5 and 20%, by weight, of ashes, between 5 and 20%, by weight, of lignin and between 55 and 90%, by weight, of holocellulose, and presented in the form of planar agglomerates of form and irregular contours, whose diameter equivalent to its projected area is essentially less than 67 mm, whose sphericity is between 0.5 and 0.9, and whose roundness is between 0.3 and 0.7, its bulk density being between 0 , 08 and 0.380 g / cm 3 .
- diameter equivalent to the area projected by the agglomerate is understood to be that diameter of the circle of the same area as that projected by the particle agglomerate in a stable position.
- Sphericity is understood as that relationship or quotient between the area of the surface of the sphere with the same volume as the agglomerate and the area of the surface of the agglomerate.
- Roundness is understood as that relationship or quotient between the perimeter of the circle with the same area as the area projected by the agglomerate in a stable position and the actual perimeter of the particle projected in a stable position.
- "Incocided" pieces of wood are understood to be not defibrated during the cooking of the wood that takes place in the process of obtaining the cellulose pulp or fiber packages that did not dissolve during said cooking.
- said fibers obtained as residues of the pulp and paper industry are the residual cellulose fibers from the industrial processes of manufacturing cellulose pulp from plant plants selected from the group that includes jute, abaca, sisal, hemp, flax, or mixtures thereof.
- said cellulose fibers from the rejections of the manufacturing processes of synthetic and textile fibers are selected from the group consisting of cellulose fibers from the rejections of the manufacturing processes of synthetic fibers.
- cellulose fibers from the rejections of the manufacturing processes of synthetic fibers eg, cellulosic fiber threads - viscose and rayon threads -, etc.
- cellulose fibers obtained from the recycling of spent textile products for example, clothing, household textiles-clothing of household-, sanitary material-bandages, dressings-, protective garments, cleaning material
- residual cellulose fibers from industrial manufacturing processes of non-woven fabrics for example, those in which non-woven fabric It is made using a hydraulic interlacing process in which jets of High speed water seals the cellulose fibers resulting in a high technical performance fabric).
- said cellulose fibers from urban and industrial solid waste are residual cellulose fibers from the urban solid waste stream (cellulose fibers from used paper and cardboard) or the residual fibers of cellulose from the recycling processes of paper and cardboard used (eg, newspaper, magazine, cartons for liquids from complex containers with plastic and aluminum, etc.), provided that, mainly, they belong to the type of Cellulose fibers indicated above, or having a length and slenderness - length / diameter ratio - similar to those of the cellulose fibers indicated above.
- the length and slenderness of the cellulose fibers, used as raw material, are preferably similar and constant within a range.
- the extent of said range depends on the characteristics of the specific embodiment of the method used to obtain the composite materials object of this invention.
- said cellulosic material (B) comprises cellulosic fibers with individual lengths between 0.1-10 mm, individual fiber diameters between 0.01-50 ⁇ m, and individual length / diameter ratios between 2-250.
- the recommended primary antioxidants are those belonging to the group of sterically hindered phenols with molecular weights greater than 300 g / mol, cinnamates, amines or mixtures thereof.
- the secondary antioxidant (E) is selected from the group consisting of phosphorus compounds, thioethers, thioesters, preferably thioethers, or mixtures thereof.
- the flame retardants (F) are selected from the group consisting of the compounds belonging to the category of phosphorus compounds, chlorinated compounds, brominated compounds or mixtures thereof.
- the flame retardants (F) indicated above can also be combined with one of the following synergistic components: aluminum trihydroxide, hydrated aluminas, borates, stannates, magnesium hydroxide, antimony oxide (III) and compounds belonging to the category of nitrogen-containing compounds.
- said composite material comprises at least one lactone.
- the composite material additionally comprises between 0.1 and 40%, by weight, with respect to the total weight of the composite material, of an additive (G) that is selected from the group formed by the stabilizers to light or UV stabilizers, modifiers of impact properties, inorganic fillers, lubricants, pigments, biocides and foaming agents or mixtures thereof.
- the additives (G) can be used to improve some of the properties and processability of the composite materials that constitute one of the objects of the present invention, provided that the final application of the composite material requires it.
- the light stabilizers are lignin, carbon black and those belonging to the groups of the bénzófeno ⁇ as, bénzotriazoles and the triazines.
- the content of said light stabilizers in the composite material can be comprised between 0.1-10%, by weight, with respect to the total weight of the composite material.
- the modifiers of the impact properties are those belonging to the group of ethylene and propylene copolymers, including grafted copolymers of ethylene and propylene, terpolymers of ethylene, propylene and non-conjugated diene monomers, and polybutenes.
- the content of said modifiers of the impact properties in the composite material may be between 1 and 30%, by weight, with respect to the total weight of the composite material.
- the lubricants are those belonging to the group of the derivatives of long main chain fatty acids, amide waxes, natural paraffins, waxes of low molecular weight polyolefins, stearates, siloxanes, and even fluorothermoplastics
- the specific lubricants to be used and their dosage levels depend on the specific production scale of the industrial process and on the specific application in which the composite materials are used.
- One of the advantages of the new composite materials according to the present invention is that they fulfill the requirements corresponding to the articles of the sectors of manufacture of electrical, electronic and telecommunications equipment.
- the formulations of the composite materials object of this invention cover the future demand for environmentally sustainable materials, due to their high content of renewable fibers and compounds that are not harmful to the environment.
- the present invention refers to a new method of obtaining the new continuous composite materials, which allows the effective use of different types of cellulose fibers (virgin or residual) for obtaining different Composite material formulations.
- Such formulations are suitable, even, for demanding applications, such as those in the manufacturing of electrical, electronic and telecommunications equipment.
- Said new method for obtaining the new composite materials with cellulosic materials comprises the following steps: a) drying the cellulosic material object of the present invention rb) providing a corroding double screw extruder, which comprises two mandrels (3), in each of which an identical spindle configuration is mounted using different spindle elements, the ratio between its external and internal diameter being between 1, 02 and 2; c) mix the components of the composite material; and d) discharge the resulting composite material through a discharge zone (4) which extends along a length between three and seven times the diameter of the extruder.
- Step a) consists in subjecting the cellulosic material to drying, preferably, to a moisture content of between 1 and 10%, by weight, for which any of the commercially available drying technologies can be used.
- an additional step may be required which comprises the transformation of the previously dried cellulosic materials into agglomerates with a size and shape suitable for continuous feeding to the equipment. of melt phase mixing in which the composite materials object of this invention are obtained.
- the cellulosic materials are transformed into planar agglomerates of irregular shape and contour, whose diameter equivalent to their projected area is essentially less than 15 mm, whose sphericity is between 0.3 and 0.7, and whose roundness is comprised between 0.1 and 0.7, suitable for continuous feeding.
- the double screw extruder used in the present invention can comprise at least two separate feeding ports and at least one degassing port and can have up to 10 openings or separate ports. Three of these ports are preferably suitable for feeding different raw materials in solid state. Four of these ports are preferably suitable for feeding raw materials in liquid phase, and the other three ports are preferably suitable for atmospheric venting, or by vacuum, of various gaseous products. This method allows the control of the length and slenderness -relation length / diameter- of the cellulose fibers, in order to optimize the properties of the composite materials that are also the object of this invention.
- step d) the resulting composite material leaves the extruder through a discharge head (5), after which it can undergo various transformation processes.
- a cord extrusion head is placed.
- the pelletizing methods are the cord granulator or the head knife granulator with air cooling or air-water mixtures.
- the composite pellet thus obtained is capable of being fed to an industrial injection molding machine in order to obtain molded products.
- the composite material after passing through the discharge zone (4) and being subjected to a granulation process, is subjected to an injection molding process.
- the composite pellets is injected at a temperature lower than 210 0 C in any of the heating zones of a chamber or plasticising cylinder of a molding machine injection.
- said composite material is subjected to a calendering process as it leaves the discharge zone (4) in order to have a thin panel, followed by compression molding.
- the composite material is subjected to a direct extrusion process after passing through the discharge zone (4).
- the necessary adjustments are made on the same extruder preparing an optimal spindle configuration for obtaining a composite material with the characteristics appropriate to each application.
- the spindle configuration chosen depends on the characteristics of the thermoplastic to be fed to the extruder (such as morphology and fluidity index) and the characteristics of the cellulosic material to be fed to the extruder (such as length and slenderness of its cellulose fibers). It also depends on the mechanical and rheological properties that the composite material to obtain must have, which, in turn, depend on the requirements of the final application in which the composite material is to be used.
- the mixing stage c) comprises the following steps: i.- dosing through a feed hopper '(6) the thermoplastic polymer (A), the agent coupling (C), the primary antioxidant (D) and the secondary antioxidant (E) and, optionally also the additives (G) that are selected from the group consisting of light stabilizers or UV stabilizers, modifiers of the impact properties, inorganic fillers, lubricants, pigments, biocides and foaming agents, by means of a set of gravimetric dosers (2), within a feeding zone of the polymer and additives (7), which comprises positive transport spindle elements and extends to The length of a length between three and seven times the diameter of the extruder; i ⁇ .- heating the mixture obtained in step i.- and transporting said mixture along a closed transport and heating zone (8) comprising positive transport spindle elements;
- fusion (9) between three and seven times the diameter of the extruder; iv.- subject the previous mixture, through the atmospheric venting port (11), to venting and degassing in a first venting zone (10) comprising spindle elements of negative or reverse transport and positive transport;
- (22) comprising spindle elements of negative or reverse transport and positive transport Ia which extends along a length between three and seven times the diameter of the extruder.
- the temperature in stage i.- is comprised between 20 and 50 0 C
- the temperature in stage i ⁇ .- is comprised between 175 0 C and 205 0 C
- the temperature in stage iii.- is between 175 0 C and 205 0 C
- the temperature in stage iv.- is between 174 0 C and 204 0 C
- the temperature in stage v.- is between 174 0 C and 204 0 C
- the temperature in stage vi.- is comprised between 173 0 C and 203 0 C
- the temperature in stage vii.- is comprised between 171 0 C and 201 0 C
- the temperature in the discharge zone (4) is comprised between 165 0 C and 195 0 C.
- each gravimetric dispenser used in stage i.- may have different configuration depending on the nature of the component to be fed: i. for pellet-shaped components, to be fed in said stage i.-, the gravimetric dispenser can preferably be selected from the double spindle feeders, whose spindles have a minimum external diameter of 20 mm, a minimum propeller angle of 11, 31 sexagesimal degrees, a minimum fillet thickness of 1.5 mm and a minimum channel depth of 3 mm; or between single spindle feeders whose spindle has a minimum external diameter of 24 mm, a minimum propeller angle of 7.12 sexagesimal degrees, a minimum fillet thickness of 1.5 mm and a minimum channel depth of 3 mm; ii.
- the gravimetric dispenser can preferably be selected from the double spindle feeders, whose spindles have a minimum external diameter of 12 mm, a minimum propeller angle of 9, 47 sexagesimal degrees, a minimum fillet thickness of 1 mm and a minimum channel depth of 1 mm; iii.
- the gravimetric dispenser can preferably be selected from the double spindle feeders , whose spindles have a minimum external diameter of 35 mm, a minimum propeller angle of 19.65 sexagesimal degrees, a minimum fillet thickness of 3 mm and a minimum channel depth of 7.5 mm.
- the spindle configuration in stage d) comprises a combination of spindle elements of positive transport and toothed mixing.
- the configuration of the gravimetric dosers used in stages v.- and viii.- will depend on the physical characteristics of the cellulosic material and the flame retardant respectively.
- the double screw gravimetric dispenser (14) used in step v.- to increase the cellulosic material can be selected from the feeders, whose spindles have a minimum external diameter of 35 mm, a minimum helix angle of 19, 65 sexagesimal degrees, a minimum fillet thickness of 3 mm and a minimum channel depth of 7.5 mm.
- the double screw gravimetric dispenser (20) used in step viii.- to feed the flame retardant has a minimum external diameter of 20 mm, a minimum propeller angle of 11, 31 sexagesimal degrees, a minimum fillet thickness of 1.5 mm and a minimum channel depth of 3 mm.
- the two mandrels of the corroding extruder preferably rotate at a speed greater than 200 rpm and the two mandrels rotate in the same direction, in accordance with the direction of transport of the components.
- a good dispersion of the cellulose fibers and the rest of the components of the composite material can be achieved.
- said speeds of rotation of the spindles allow to achieve productions of composite material higher than those that can be achieved, using the embodiments described in the prior art.
- the method object of the invention allows, however, the control of the length and slenderness -relation length / diameter- of the cellulose fibers, in order to optimize the properties of the composite materials, according to the applications that are also object of this invention.
- stage vi.- said cellulosic material is kneaded with the components of the composite material that have been mixed and kneaded in the previous stages.
- the cellulosic material is subjected to dispersive or distributive mixing, depending on the spindle elements selected, in accordance with the spindle configuration chosen to obtain the composite material.
- stage vi.- comprises kneading by means of toothed mixing elements. This configuration allows the fibers to be distributed evenly and effectively.
- Stage ix.- of flame retardant kneading You should understand as little time as possible to prevent additives that can decompose due to shearing, such as some flame retardants, from decomposing.
- the composite materials according to the present invention have characteristics that make them suitable for use in the manufacture of components for various sectors, even for moderately demanding applications, such as those in the sectors of manufacture of electrical, electronic and telecommunications equipment, being able to in this way replace different materials reinforced with fiberglass and thermosetting polymers, currently used. Among these requirements are resistance to abnormal heat and fire. Moreover, the composite materials according to the present invention respond to the growing environmental restrictions, by reusing waste materials from other industries. An important advantage is that the new composite materials have a uniform rheological behavior and a relatively low viscosity that makes them easily moldable in various articles, following different techniques such as extrusion, injection molding and compression molding, using the machinery available in the market. This advantage is inherent in the new composite materials and the method object of the present invention.
- the present invention relates to the use of the composite material according to the present invention to obtain molded articles.
- Said articles are especially suitable for use in the electrical, electronic and telecommunications sectors, preferably for the manufacture of fuse bases, common telecommunications infrastructures and boxes for meter centralization.
- the articles obtained meet the requirements of stability and resistance to heat and fire required in these industries.
- said articles formed from a composite material according to the present invention are also suitable for use in the construction, aviation, automotive, furniture sectors.
- ETP Positive Transport Element
- EA Kneading Element
- ETN Negative Transport Element
- EMD Serrated Mix Element
- a composite material was obtained which, for every 100 parts of its weight, comprised:
- the composite material pellet of the formulation corresponding to this example, finally obtained, was fed to an injection molding machine of 450 kN of closing force, in which the cylinder or plasticizing chamber of the injection molding machine is heated according to the selected temperature profile (see table III):
- the cooling time was 25 seconds.
- multipurpose specimens were obtained in accordance with ISO 3167 that were used to determine the properties of the composite material obtained.
- the values of the main mechanical and thermal properties of the composite materials obtained were:
- Example 2 Following the method described in Example 1 and using planar agglomerates of a cellulosic material consisting of virgin fibers of raw cellulose pulp of Eucalyptus globulus previously dried and whose morphology allowed its continuous feeding to the extruder without being subjected to the aforementioned transformation process, a composite material was obtained which, for every 100 parts of its weight, included:
- the composite material pellet of the formulation corresponding to this example was injected to obtain multipurpose specimens in accordance with ISO 3167. According to ISO standards, the values of the main mechanical properties and The thermal materials obtained were (see table IV):
- pellets were produced in sufficient quantity to feed an industrial injection molding machine of 2000 kN of closing force, in which the cylinder or Plasticizing chamber of the injection molding machine was heated according to the following selected temperature profile (see Table VII):
- pellets were produced in sufficient quantity to feed an industrial injection molding machine of 800 kN closing force, in which the cylinder or Plasticizing chamber of the injection molding machine was heated according to the temperature profile, selected as follows (see table IX):.
- the cooling time was 12 seconds.
- the body and the handle of the fuse holder base for cylindrical fuses are shown, which is shown in Figure 4, characterized by a minimum wall thickness of 2 mm and for whose injection the maximum melt flow path was 25 cm, approximately.
- This product underwent various tests set by the standards that apply to these types of products.
- Table X shows the results of said tests, as well as their comparison with the results obtained for the same product manufactured with a conventional material such as poly (butylene glycol terephthalate) (PBTP) reinforced with 30% fiberglass.
- PBTP poly (butylene glycol terephthalate)
- pellets were produced in sufficient quantity to feed an industrial injection molding machine of 800 kN closing force, in which the cylinder or Plasticizing chamber of the injection molding machine was heated according to the following selected temperature profile (see table Xl):
- the cooling time was 8 seconds.
- the body and the handle of a fuse holder base for cylindrical fuses were manufactured similar to that shown in Figure 4, characterized by a minimum wall thickness of 1.74 mm and for whose Injection, the maximum melt flow path was approximately 20 cm.
- This product underwent various tests set by the standards that apply to these types of products.
- Table XII shows the results of said tests, as well as their comparison with the results obtained for the same product manufactured with a conventional material such as poly (butylene glycol terephthalate) (PBTP) reinforced with 30% fiberglass.
- PBTP poly (butylene glycol terephthalate)
- pellets were produced in sufficient quantity to feed an industrial injection molding machine of 5000 kN of closing force, in which the cylinder or Plasticizing chamber of the injection molding machine was heated according to the following selected temperature profile (see table XIII): Table XIII
- the cooling time was 60 seconds.
- a part of the body of the closed three-pole vertical bases was shown, which is shown in Figure 5, characterized by a minimum wall thickness of 1.66 mm and for whose injection the maximum melt flow path was 48 cm, approximately.
- This product underwent various tests set by the standards that apply to these types of products.
- Table XIV shows the results of said tests, as well as their comparison with the results obtained for the same product manufactured with a conventional material such as pqljar ⁇ ida. reinforced with 20% fiberglass.
- D ext means external diameter of each spindle; ⁇ means the propeller angle of each spindle; Esp. Means thickness of the fillets of each spindle; Prof. means Channel depth of the channels of each spindle; D hEmb means external diameter of the spindles of the stuffer.
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Abstract
La présente invention concerne des matériaux composés comprenant des fibres de cellulose et des polymères thermoplastiques, un procédé de production en continu desdits matériaux composés et l'utilisation desdits matériaux composés dans la fabrication de divers articles moulés.
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ES200600541A ES2281290B1 (es) | 2006-03-06 | 2006-03-06 | Material compuesto, metodo para su produccion en continuo y uso del mismo. |
ESP200600541 | 2006-03-06 |
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WO2019055921A3 (fr) * | 2017-09-15 | 2019-04-25 | Hamilton Robert T | Matériaux composites cellulosiques |
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ES2322928B1 (es) * | 2007-07-26 | 2010-04-23 | Condepols, S.A. | Procedimiento para la elaboracion de perfiles por extrusion de materiales compuestos. |
FI20216326A1 (en) * | 2021-12-22 | 2023-06-23 | Fortum Oyj | Composite product and uses thereof |
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US4339363A (en) * | 1979-07-05 | 1982-07-13 | Kabushiki Kaisha Mikuni Seisakusho | Composite material compositions using wastepaper and method of producing same |
US5088910A (en) * | 1990-03-14 | 1992-02-18 | Advanced Environmental Recycling Technologies, Inc. | System for making synthetic wood products from recycled materials |
WO1999056936A1 (fr) * | 1998-05-07 | 1999-11-11 | Instituut Voor Agrotechnologisch Onderzoek (Ato-D Lo) | Procede de production en continu de composites de polymere et de fibres cellulosiques et materiaux composes ainsi obtenus |
WO2006108256A1 (fr) * | 2005-04-13 | 2006-10-19 | Ford Motor Company Brasil Ltda. | Materiel destine a un moulage par injection, son procede, et son utilisation |
-
2006
- 2006-03-06 ES ES200600541A patent/ES2281290B1/es not_active Expired - Fee Related
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2007
- 2007-03-06 WO PCT/ES2007/000117 patent/WO2007101896A1/fr active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US4339363A (en) * | 1979-07-05 | 1982-07-13 | Kabushiki Kaisha Mikuni Seisakusho | Composite material compositions using wastepaper and method of producing same |
US5088910A (en) * | 1990-03-14 | 1992-02-18 | Advanced Environmental Recycling Technologies, Inc. | System for making synthetic wood products from recycled materials |
WO1999056936A1 (fr) * | 1998-05-07 | 1999-11-11 | Instituut Voor Agrotechnologisch Onderzoek (Ato-D Lo) | Procede de production en continu de composites de polymere et de fibres cellulosiques et materiaux composes ainsi obtenus |
WO2006108256A1 (fr) * | 2005-04-13 | 2006-10-19 | Ford Motor Company Brasil Ltda. | Materiel destine a un moulage par injection, son procede, et son utilisation |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2019055921A3 (fr) * | 2017-09-15 | 2019-04-25 | Hamilton Robert T | Matériaux composites cellulosiques |
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