CN117580896A - Cellulosic fibrous material and method - Google Patents
Cellulosic fibrous material and method Download PDFInfo
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- CN117580896A CN117580896A CN202280046194.1A CN202280046194A CN117580896A CN 117580896 A CN117580896 A CN 117580896A CN 202280046194 A CN202280046194 A CN 202280046194A CN 117580896 A CN117580896 A CN 117580896A
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Landscapes
- Reinforced Plastic Materials (AREA)
Abstract
The present invention relates to a cellulosic fibrous substrate comprising at least one top surface and at least one bottom surface. The cellulosic fibrous substrate further comprises 60 to 90wt% cellulosic fibers having a length of at most 10mm, 0 to 10% acid cure catalyst, and 10 to 40wt% binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof.
Description
Technical Field
The present invention relates to cellulosic fibrous thermosets and methods of making the cellulosic fibrous thermosets.
Background
In view of the growing awareness of the negative environmental impact on global warming and marine and soil pollution, it is necessary to replace pure fossil-based plastics, mineral filled plastics and Fiber Reinforced Plastics (FRP), glass Fiber Reinforced Plastics (GFRP) and carbon reinforced plastics (CFRP) with more environmentally friendly alternatives. FRP composites, such as GFRP and or CFRP composites, exhibit high or very high strength to weight ratios and are extremely rigid due to the significant length and strength of the man-made non-degradable fibers. These FRP composites are often used in a variety of applications where, for example, flexural strength, impact resistance and/or weatherability are important, such as in vehicles, in sports equipment, construction, electrical housings, and the like. However, the environmental impact of these materials is high in terms of the manufacture of raw materials such as glass or carbon fiber, the production of intermediates thereof, and the handling and/or recycling thereof. More environmentally friendly alternatives, such as bio-based or bio-based polymers, have been tried to replace fossil-based polymers in GFRP and CFRP materials. Further, attempts have been made to replace glass or carbon fibers with natural fibers such as flax, hemp, sisal, and the like. However, the main challenges of biobased and/or biofouling substitutes and renewable and/or natural fiber substitutes for GFRP and CFRP composites are high price, lack of sufficient quantity and quality consistency of supplies that can compete with fossil-based polymers and rayon.
Natural Fiber Composites (NFC) are classified into non-wood fiber based composites, wood fiber and wood particle based composites. Wood fibers are generally shorter in length than other natural fibers such as jute or flax. Because of the longer length of non-wood fibers (natural fibers), the potential is greater than, for example, wood fibers and/or wood particles in bend-strength driven applications. These fibers typically have high (> 50%) cellulose, have a high propensity for hydrophilicity, and create problems such as natural decay processes, dimensional instability, delamination, and other problems due to climatic cycling (humidity and temperature). To address these problems, the NFC industry needs to saturate the composite with binders, such as thermosets and thermoplastics, which are typically fossil based, in which case >20% of the biomass content (drive) is considered high in such systems. This means that combining these natural fibers with fossil-based systems is harmful to the environment and recycling or separation is also very problematic.
In pulp and paper production, a large and stable renewable resource of cellulose fibers is from the foster industry company (Forrest industries) from different wood species such as conifer or eucalyptus. Recently, many NFC materials have been produced that combine cellulosic fibers and polymers from forests to reduce environmental impact and also produce load bearing articles. Such materials are typically manufactured by mixing and compounding pure wood fibers or fibers from pulp and paper production into particles for injection molding, wherein the final product is therefore not based on laminar sheets.
A well-known solution to create a cellulose fiber based carrying 3D single-bent or expandable solution is a wood veneer comprising layers, wherein long wood fibers in each layer are placed generally perpendicular to the wood fibers in the adjacent layers, and wherein the layers are hot pressed into a single-bent shape, such as the seat of a chair. For more complex 3D surfaces, such as hyperbolic or non-developable surfaces, special and expensive 3D veneers or plastics are the only choice, as conventional veneers tear and break when trying to create a hyperbolic surface.
Another well known example of the use of short cellulose fibers found in paper is the use of high pressure laminates or HPLs consisting of several different layers of paper and surface material and a polymer or phenolic binder to create flat load bearing applications. While some special and singular grades of HPL may be post-formed around a single curved edge by applying heat and constraints and using thermoplastic adhesives that can be post-formed, HPL has never been used to make articles with complex 3D non-deployable surfaces (including single curved, double curved and/or combinations of rotation and translation), such as bearing spheres for helmets, cylindrical rotating surfaces for vases, or complex surfaces for ship hulls.
In both of the above examples, indoor use is the intended use, as natural fibers are hydrophobic and/or degraded with UV. In the case of HPL, the outermost layer typically has a special coating for improved scratch resistance, UV resistance and moisture resistance as well as a decorative appearance, such as imitation of marble or wood. Such a material may be used, for example, as a stack of counter tops or laminate floors.
Another option for creating a complex 3D carrier article comprising layers of fibers from renewable natural sources and having high tensile and flexural strength is to use cellulosic fibers such as hemp, flax, ramie and sisal. Such fibers may be woven into a still flat 2D flexible mat/fabric impregnated with adhesive. These materials are often used to provide flat 3D structures with advantageous mechanical properties. Here, the length of the fibers is critical, where each fiber is placed on a complex 3D surface. This process is expensive and the source of harvested fiber is competing with the food and textile industries. Another challenge is that long natural fibers are hydrophilic, thus absorbing moisture and making them unsuitable for outdoor use and wet spaces. In addition, the need for polymeric binders also makes such natural fiber composites, like any composite containing a polymer, difficult or impossible to recycle, thereby disrupting the plastic recycling cycle.
Finally, it is known to combine cellulosic fibres with polymeric materials such as thermoplastics in order to manufacture granules for injection moulding, extrusion and blow moulding and compression moulding. While thermoplastic materials can be bio-based and biodegradable, such materials are quite expensive and bio-based solutions are not as characteristic as fossil-based resin systems. Moreover, the debate as to whether NCF and bio-based polymers (which in turn are based on field-grown crops) would compete with the agricultural land required for food production is continuing. Furthermore, in several cases the need for fertilizers and low yields have shown that so-called bioplastics have a negative impact on the overall environment. In addition, weather uncertainty affects the collection year by year, thereby producing price fluctuations.
In view of the challenges presented in the current art, it is desirable to provide cellulosic fibrous substrates that contain natural and renewable components with low environmental impact while achieving mechanical properties comparable to fibrous composites such as GFRP, fossil based polymers, and even metals such as aluminum. Further, it is desirable to provide materials and methods for obtaining such substrates. And creating a solution for mass production by: 1) The use of stable and process-based large-scale non-food competitive bio-based raw material sources 2) creates characteristics that enable highly automated production processes by reducing problems such as difficulty in incorporating wet and viscous solutions for internal logistics, robotic systems, etc., which are often the case with manual reinforced fiber composite solutions on the market.
Disclosure of Invention
In view of the above, the present invention is directed to solving at least some of the problems/voids in the prior art. To this end, the invention provides cellulosic fibrous materials and methods for producing the same. Cellulosic fibrous materials based on renewable natural resources comprise a surface, wherein the surface has at least one expandable and/or non-expandable surface portion.
The cellulose fiber substrate according to the present invention comprises at least one top surface, at least one bottom surface, and is characterized in that the cellulose fiber substrate further comprises 60 to 90wt% of cellulose fibers having a length of at most 10mm, 0 to 10% of an acid curing catalyst, and 10 to 40wt% of a binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof.
In one embodiment, a cellulosic fibrous substrate is provided wherein the binder is polyfurfuryl alcohol (PFA).
In one embodiment, a cellulosic fibrous substrate is provided wherein the cellulosic fibers comprise from 0 to 100% virgin cellulosic fibers and from 0 to 100% recycled cellulosic fibers.
In one embodiment, a cellulosic fibrous substrate is provided wherein the at least one top and/or bottom surface has at least one expandable and/or non-expandable surface portion.
In one embodiment, a cellulosic fibrous substrate is provided, wherein the cellulosic fibers are arranged substantially parallel in the substrate, or wherein the cellulosic fibers are arranged substantially cross-wise in the substrate, or wherein the cellulosic fibers are arranged substantially randomly or in a combination thereof in the substrate.
In one embodiment, a cellulosic fibrous substrate is provided wherein the substrate comprises at least one cavity.
The load-bearing 3D article according to the invention comprises a cellulosic fibrous substrate according to the invention.
In one embodiment, a load bearing 3D article is provided, wherein the load bearing article has a tensile strength of at least 40MPa, preferably at least 50MPa, more preferably at least 100 MPa.
In one embodiment, a carrier 3D article is provided, wherein the carrier article has a thickness of at least 2.5mm, preferably at least 5mm, more preferably at least 10mm.
A method for manufacturing a cellulosic fibrous substrate comprising at least a top surface and a bottom surface according to the present invention comprises the steps of:
a) Providing at least one sheet of cellulosic fibers having a maximum length of 10 mm;
b) Impregnating the at least one sheet of cellulose fibers with a mixture of an acid curing catalyst and a binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof;
c) Pre-curing the sheet of at least one impregnated cellulose fiber by heating in the range of 50 ℃ to 300 ℃ to obtain a prepreg;
d) Disposing one or more prepregs into a stack;
e) The stack is pressed in a pressing tool with a pressure of at least 7kg/cm2, preferably at least 25kg/cm2, more preferably at least 30kg/cm2 and a temperature of at least 60 ℃, preferably at least 140 ℃, more preferably at least 150 ℃ for a period of at least 10 seconds, preferably at least one minute, more preferably at least two minutes, so as to obtain a cellulosic fibrous substrate having at least one top surface and one bottom surface.
In one embodiment, a method for making a cellulosic fibrous substrate is provided wherein the binder is polyfurfuryl alcohol (PFA).
In one embodiment, a process for making a cellulosic fibrous substrate is provided wherein the cellulosic fibers comprise a mixture of 0-100% virgin cellulosic fibers and 0-100% recycled cellulosic fibers.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, wherein cellulosic fibers are provided in the form of paper.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided wherein the top surface and/or the bottom surface has at least one expandable and/or non-expandable surface portion.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, wherein the cellulosic fibrous substrate has a biobased carbon in an amount of at least 80%.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, wherein the cellulosic fibrous substrate comprises from 60 to 90wt% of the cellulosic fibers.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, wherein the cellulosic fibrous substrate comprises 10 to 40wt% of the binder.
In one embodiment, a process for manufacturing a cellulosic fibrous substrate is provided, wherein the cellulosic fibrous substrate comprises from 0 to 10wt% of the acidic catalyst.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided wherein the prepregs in the stack are oriented such that the directions of the textures in the prepregs are substantially parallel.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided wherein the prepregs in the stack are oriented such that the angle of the grain direction in the prepregs is in the range of 0-90 ° relative to the adjacent prepregs.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, further comprising a step f) of cutting the prepreg and/or the cellulosic fibrous substrate into a predetermined shape.
In one embodiment, a method for manufacturing a cellulosic fibrous substrate is provided, further comprising step g) of creating a cavity in the cellulosic fibrous substrate.
Further features of, and advantages with, the present invention will become apparent when studying the appended claims and the following description. Those skilled in the art will recognize that different features of the invention can be combined to create embodiments other than those described in the following without departing from the scope of the invention.
Drawings
These and other aspects of the invention will now be described in more detail, with reference to the appended drawings showing embodiments of the invention wherein:
FIGS. 1a-1c depict examples of surfaces of a cellulosic fibrous substrate according to the present invention;
FIGS. 2a-2e show another example of a surface of a cellulosic fibrous substrate according to the present invention;
FIG. 3a shows three layers of prepreg material and FIG. 3b shows a cured cellulosic fibrous substrate shaped into a curved surface;
FIG. 4 shows an example of a cellulosic fibrous substrate of the present invention;
FIG. 5 depicts a tensile strength test of a cellulosic fibrous substrate;
fig. 6 shows comparative data for tensile strength of the cellulosic fibrous substrate analyzed in fig. 5 relative to other materials.
Fig. 7 shows a temperature diagram during the pressing step according to the invention.
Fig. 8 shows a cross section of a substrate according to the invention.
Detailed Description
The present invention will now be described below with reference to the accompanying drawings, in which exemplary embodiments of the invention are shown. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments of the invention are provided by way of example so that this disclosure will convey the scope of the invention to those skilled in the art. In the drawings, the same reference numerals refer to the same or similar components having the same or similar functions, unless otherwise specifically indicated.
As described above, the cellulose fiber substrate contains cellulose fibers having a length of at most 10mm. Cellulose fibers are made from ethers or esters of cellulose, which can be obtained from bark, wood or leaves of plants or other plant-based materials. The cellulosic fibers may originate from the conversion of wood to wood pulp. The length of each cellulosic fiber in the composite may be the same as or different from the length of the other cellulosic fibers. Indeed, it is conceivable that some of the cellulose fibers may have a length of more than 10mm, but the amount of these fibers should be considered negligible. The term "negligible" is understood to mean an amount of less than 0.01% by weight. The cellulosic fibers may be provided in any suitable form such as sheet, roll, batt, or the like.
The cellulose fibers that can be used to make the cellulose fiber substrates according to the present invention can be recycled cellulose fibers, which provides the advantages of reducing the cost of the cellulose fiber substrates and contributing to the recycling economy. On the other hand, the cellulose fibers may be virgin cellulose fibers that provide increased tensile and/or flexural strength of the circuit board compared to when recycled cellulose fibers are used. Further, it is conceivable that the cellulose fibers are a mixture of recycled cellulose fibers and virgin cellulose fibers, which ranges from 0 to 100% virgin cellulose fibers and from 0 to 100% recycled cellulose fibers, respectively. The cellulosic fibers may include paper, such as softwood kraft paper, hardwood kraft paper, sulfite fibers, organic solvent fibers, nonwovens, or combinations thereof. It is envisioned that cellulose fibers comprise 50 to 90wt% of kraft paper. The paper may be provided in the form of a sheet and/or in the form of a continuous sheet, such as a paper roll.
The cellulosic fibrous substrate of the present invention may comprise 40 to 90wt% cellulosic fibers and 10 to 40wt% binder. The cellulosic fibrous substrate may have biobased carbon in an amount of at least 80%, preferably at least 90%, more preferably at least 95%. The bio-based carbon is derived in whole or in part from biomass resources. Biomass resources are organic materials that are available on a renewable or recurring basis, such as crop residues, wood residues, grasses, and aquatic plants. In contrast, non-bio-based carbon is made entirely from petrochemical resources. The amount of biobased carbon referred to above is a measure of the amount of biobased carbon in the product compared to the sum of biobased carbon and petroleum based carbon in the product. The term biobased carbon describes carbon of non-fossil origin and relates to cellulosic fibres and/or binders and/or additives.
The cellulosic fibrous substrate according to the present invention further comprises a binder selected from the group consisting of: cellulose, hemicellulose, lignin, furan, preferably polyfurfuryl alcohol (PFA), and combinations thereof.
The cellulosic fibrous substrate may contain additives such as catalysts, UV agents, conductive compounds, pigments, hydrophobic substances, softeners, hardeners, curing agents, and the like. The catalyst may be an acidic catalyst, such as an inorganic or organic acid. The catalyst may be added in the range of 0-10wt% and may have a pH of <5 and/or an acid number of <5mg KOH/g. Additives may be added to improve chemical resistance, fire resistance and abrasion resistance, and/or to increase the cure speed, thereby maximizing production.
The prepreg material of the present invention unexpectedly shows advantageous floating properties during the curing step, which is likely due to the combination of relatively short fibers with a binder having a certain viscosity. It is conceivable to add alcohols in the process, for example a maximum of 20% ethanol or methanol, to further improve the buoyancy. The term floating is understood to be the property of cellulose fibers to be able to migrate and fill in cracks and tears that may occur during the manufacture of the cellulose fiber substrate. The floating properties enable the cellulose fibers to adapt to the shape of the mold or tool during the manufacturing process. As shown in fig. 1-4, the floating properties enable the fabrication of complex shapes such as 3D shapes as well as flat surfaces and provide control over the micro-surface structure, thereby enabling the custom fabrication of additional properties such as surface properties, e.g., smooth and blank or matte and roughened surfaces. It is envisioned that shapes made in accordance with the present invention may be flat, single curved, double curved, spherical, compound (complexes) or have holes therein. Figures 3a and 3b show how a single sheet of prepreg is deformed into a single homogeneous material of curved configuration. Fig. 8 shows a cross section through a cellulosic fibrous substrate, it being impossible to distinguish between individual cellulosic fibrous layers used during the manufacturing process. In the manufacturing process according to the invention, the short fibers are made possible by their unexpected floating effect. Fig. 3a shows an embodiment in which the cellulosic fibrous substrate is made from three prepreg layers. Each of the prepreg layers contains cellulose fibers and a binder as described above. The layers are of equal thickness.
As described above, the cellulosic fibrous substrate comprises a surface, wherein the surface has at least one expandable and/or non-expandable surface portion. Figures 1a-1c illustrate different examples of such surfaces. In particular, fig. 1a shows a malleable or single curved surface, while fig. 1b and 1c depict a non-malleable or double curved surface.
Fig. 2a-2e illustrate another example of a surface comprising expandable and non-expandable surface portions. Fig. 2a is a perspective view of such a surface, while fig. 2b and 2c are front and top views, respectively. As can be seen in fig. 2d and 2e, the surface depicted in fig. 2a contains non-expandable portions a and B.
In the context of the present invention, a spreadable surface is a smooth surface with zero gaussian curvature. Gaussian curvature is defined as the product of two principal curvatures of a surface. In other words, a deployable surface is a non-planar surface that can be flattened onto a plane without deformation, i.e., it can bend without stretching or compressing. Conversely, it is a surface that can be made planar by converting it by folding, bending, rolling, cutting and/or gluing. Examples of expandable surfaces are cylinders and cones.
In contrast, a non-developable surface is a surface with a non-zero gaussian curvature. Thus, a non-expandable surface is a non-flat surface that cannot be flattened onto a plane without deformation. Most surfaces are typically non-developable surfaces. The non-developable surface may be referred to as a hyperbolic surface. One of the most common non-expandable surfaces is a sphere.
Fig. 4 shows a cellulosic fibrous substrate according to the invention, wherein the cellulosic fibrous substrate is a chair seat. As can be seen in fig. 4, the chair seat comprises four sections C-F, which will be described in more detail below.
Part C contains a complex non-expandable 3D surface that contains edges with an arc shape and a transition from a hyperbolic surface to a singly curved surface. Part D comprises a non-developable complex 3D surface comprising edges having an arc shape and a transition from a polar hyperbolic surface to a polar monocurved surface. Turning attention to point E, a complex 3D edge is shown that contains a larger radius with a hyperbolic surface (i.e., a non-developable surface). Part F includes complex 3D edges where sharp edge radii (sharp edge radius) (r <2 mm) are maintained along all transitions between the single curved surface and the double curved surface.
The cellulosic fibrous substrate of the present invention may have at least one portion comprising a radius of curvature of less than 10cm, preferably less than 5 cm.
Cellulose fibers are made from ethers or esters of cellulose, which can be obtained from bark, wood or leaves of plants or other plant-based materials. The cellulosic fibers may originate from the conversion of wood to wood pulp. The length of each cellulosic fiber in the cellulosic fiber substrate may be the same as or different from the length of the other cellulosic fibers. Indeed, it is conceivable that some of the cellulose fibers may have a length of more than 10mm, but the amount of these fibers should be considered negligible. The term "negligible" is understood to mean an amount of less than 0.01% by weight. The cellulosic fibers may be provided in any suitable form such as sheets, pellets, and the like.
The cellulose fibers may be randomly oriented or may be oriented such that the longitudinal extensions of the fibers are substantially parallel.
The cellulosic fibrous substrate of the present invention may comprise 40 to 90wt% cellulosic fibers and 10 to 40wt% binder. The cellulosic fibrous substrate according to the present invention further comprises a binder selected from the group consisting of: thermoset resins, reactive thermoplastic resins, cellulose, hemicellulose, lignin, bio-based polymers, and combinations thereof. The thermosetting resin may be substituted and unsubstituted furan, epoxy, polyurethane or phenolic resin. The reactive thermoplastic resin may have similar properties to the thermosetting resin after curing and may be in liquid or powder form. Such binders are readily available, cost effective, generally biodegradable, and environmentally friendly. In particular, the binder is polyfurfuryl alcohol (PFA). Among the bio-based polymers, mention may be made of polylactic acid, poly-L-lactide, polyhydroxybutyrate, polyhydroxyalkanoate (PHA), polyamide, polypropylene (PP) and polyethylene terephthalate.
As described above, it was unexpectedly found that while the stack of prepregs constituting the cellulosic fibrous substrate of the invention comprises layers, the final cellulosic fibrous substrate according to the invention is considered to be made from a homogeneous cellulosic fibrous substrate, as illustrated in fig. 3b and 7. Without wishing to be bound by theory, it is believed that this effect is achieved due to the length of the cellulose fibers being below 10mm, preferably below 4 mm. As mentioned above, the short hydrophilic cellulose fibers are substantially completely impregnated with the binder. Further, when the stack of prepregs is subjected to high pressure and formed into a cellulosic fiber substrate, little cracks form because the cellulosic fibers can be rearranged due to the short fiber length without breaking. Further, even if a crack occurs in one layer of the stack of prepregs, it can be filled with cellulose fibers from at least one adjacent layer of the stack of prepregs. Fig. 8 shows a cross section through a cellulosic fibrous substrate, it being impossible to distinguish between individual cellulosic fibrous layers used during the manufacturing process. In the manufacturing process according to the invention, the short fibers are made possible by their unexpected floating effect.
The cellulosic fibrous substrate according to the invention has a tensile and/or flexural strength of at least 40MPa, preferably at least 50MPa, more preferably at least 100 MPa. Those skilled in the art will immediately appreciate that such tensile and/or flexural strength is highly unexpected for articles comprising cellulosic fibrous substrates based on short cellulosic fibers. Such high tensile and/or flexural strength exceeds the tensile and/or flexural strength of articles comprising wood and plastic based cellulosic fibrous substrates and is comparable to the tensile and/or flexural strength obtained when using certain cellulosic fibrous substrates.
The mechanical properties of the substrates according to the invention were measured as follows:
fig. 5 shows the results of the tensile strength test according to ISO 527. Six different samples with different thicknesses were tested. As can be seen from the table shown in fig. 5, the average tensile strength was measured to be 166MPa, which significantly exceeded the tensile strength of wood and woody materials, and was comparable to porous ceramics and composites such as GFRP (fig. 6).
One of the reasons for the high tensile and/or flexural strength of the cellulosic fibrous substrates of the present invention is believed to be good adhesion between the fibers and the binder. The binder aids in the internal mechanical crosslinking of the fibers to one another such that the fibers are trapped and locked in one another, thereby aiding the tensile and/or flexural strength of the cellulosic fibrous substrate.
Another reason for the high tensile and/or flexural strength of cellulosic fibrous substrates is the possibility to determine the fiber orientation in 3D articles during manufacture.
The cellulose fibers may be randomly oriented or may be oriented such that the longitudinal extensions of the fibers are substantially parallel or substantially intersecting. To this end, the fibers may be positioned such that the longitudinal extensions (grain directions) of the main portions of the fibers are aligned in the same direction. This may be achieved by arranging one or more prepregs in a stack in a particular direction. In particular, at least one prepreg may be oriented such that the direction of the texture of the cellulose fibers in the at least one prepreg is substantially parallel to the direction of the texture of the cellulose fibers of another one of the at least one prepreg. It has been shown that the tensile and/or flexural strength in the direction parallel to the grain direction is significantly higher, for example up to twice as high, than the tensile and/or flexural strength in the direction perpendicular to the grain direction. Thus, the cellulosic fibrous substrate may be designed such that the tensile and/or flexural strength is suitable for the intended use.
The cellulose fibers of each of the at least one prepreg may also be oriented such that the cellulose fibers are arranged in a cross shape. The at least one prepreg may then be arranged such that the direction of the texture of the cellulose fibers of one of the at least one prepreg is perpendicular to the direction of the texture of the cellulose fibers of the other of the at least one prepreg. The at least one prepreg may also be arranged such that the direction of the texture of the cellulose fibers of one of the at least one prepreg is at an angle of 0-90 ° to the direction of the texture of the cellulose fibers of the other of the at least one prepreg, thereby achieving a cross shape having an angle ranging from zero to right angles.
It is known that cellulosic fibrous substrates comprising cellulosic fibers such as hemp, flax, ramie and sisal can exhibit relatively high tensile and/or flexural strength. It has been unexpectedly found that the 3D articles of the present invention comprising a cellulosic fibrous substrate comprising short cellulosic fibers (i.e. cellulosic fibers having a length of at most 10mm, preferably at most 4 mm) exhibit comparable tensile and/or flexural strength as a natural cellulosic fibrous substrate having long cellulosic fibers. Meanwhile, due to the fact that the short cellulose fibers are impregnated with the binder, the article comprising the short cellulose fibers becomes waterproof to a greater extent than the article comprising the long cellulose fibers. The term "waterproof" means hydrophobic and/or having a density that prevents penetration of water through the material. Because the short cellulose fibers are easily moved within the cellulose fiber substrate during manufacture, the layers are enabled to fuse because the fibers can "float" and fill in cracks and tears that may occur during manufacture of cellulose fiber substrates having complex surface structures. According to the present invention, a cellulosic fibrous substrate having a small radius of curvature, which is a known problem in the art of creating complex 3D structures, can be manufactured.
The cellulose fiber substrates according to the invention exhibit high moisture resistance due to the nature of the binder in combination with the possible combination of the production process. Further, it has been found that the cellulosic fibrous substrate according to the present invention is self-extinguishable when PFA is used.
Further, it has been found that the cellulosic fibrous substrate according to the present invention is flammable and self-extinguishable. According to the glow wire test according to IEC 60695-2-12:2021, the cellulosic fibrous substrate according to the invention passes the temperature test of 650℃and 850℃when cured with PFA as binder. The cellulose fiber substrates according to the invention are fire-resistant according to STD 104-0001/ISO 3795, UV-resistant according to STD 423-0061, scratch-resistant according to STD 423-0030, heat-resistant according to Volvo STD 423-0055, impact-resistant according to EN 13087 and VOC-free according to Volvo STD 429-0003. The cellulosic fibrous substrate according to the invention has a density of 1.34g/cm measured according to ISO 11183 3 The glass transition temperature Tg measured according to ISO 11358 is 145℃and the Charpy impact strength measured according to ISO 179 is 8.6kJ/m 2 . The life cycle analysis of the cellulosic fibrous substrate according to the invention calculated 0.65kg CO 2 -equivalent weight.
Examples of cellulosic fibrous substrates of the present invention are sports equipment such as helmets and skateboards, furniture such as chairs and tables, and vehicle parts such as dashboards, door handles and interior trim. Further, the cellulose fiber substrate can be used for architectural design and construction, consumer electronics, large household appliances, and the like.
Thus, the cellulosic fibrous substrate of the present invention can replace the cellulosic fibrous substrates currently available that contain more expensive and less environmentally friendly materials such as plastics and GFRP, without compromising tensile and flexural strength and even improving tensile and flexural strength compared to plastics and wood.
The cellulosic fibrous substrates of the present invention have a high moisture resistance, which is very beneficial when the cellulosic fibrous substrates are intended for outdoor use or for use in humid environments such as bathrooms, or for use in humid climates. Further, the finishing of the surface of the cellulosic fibrous substrate of the present invention is highly decorative and aesthetically attractive and can be further adapted for the desired application. In particular, the surface of the cellulosic fibrous substrate may be glossy or dull. The cellulosic fibrous substrate may have a gloss-satin finish, a matte finish, a roughened surface, a patterned surface, or a surface having text or graphics thereon. The cellulosic fibrous substrate and 3D articles made therefrom according to the present invention may have different thicknesses throughout the detail, or the same thickness throughout the detail.
The thickness of the cellulosic fibrous substrate according to the invention and the 3D article made therefrom may be at least 1.5mm, preferably at least 2.5mm, preferably at least 5mm, more preferably at least 10mm. As is evident from the above, the cellulosic fibrous substrate of the present invention exhibits unprecedented strength despite a relatively low thickness. The cellulosic fibrous substrate thus combines a low weight and slim structure with a high impact strength. The cellulosic fibrous substrate according to the present invention and 3D articles made therefrom may also have a significantly greater thickness, such as a thickness of at least 20mm, preferably at least 40mm, more preferably at least 50 mm. Further, the cellulosic fibrous substrate may have a total surface area of at least 0.1m 2 . In particular, the total surface area of the cellulosic fibrous substrate may be 0.3m 2 To 100m 2 . In other words, the cellulosic fibrous substrate can be quite large and still exhibit unprecedented strength, which enables the use of such articles for impact absorbing applications.
The cellulosic fibrous substrate of the present invention may be rigid. The term "rigid" is intended in the context of the present invention to mean either lack of flexibility or lack of flexibility. The cellulosic fibers in the cellulosic fiber substrate may be provided in the form of a sheet.
The cellulosic fibrous material from which the 3D articles of the present invention are made may be in the form of at least one cellulosic fibrous layer impregnated with a binder. Further, the cellulosic fibrous substrate from which the 3D article of the invention is made may be a stack of prepregs comprising at least two layers, preferably at least three layers. The term "stack of prepregs" is understood to mean a product made by laminating a stack of one or more materials, i.e. by combining them. In practice, the stack of prepregs may comprise more than three layers, for example at least four layers, preferably at least five layers and more preferably at least six layers. Each layer preferably comprises cellulosic fibres as described above and a binder.
It has unexpectedly been found that while the stack of prepregs comprising the cellulosic fibrous substrate of the invention comprises layers, the final cellulosic fibrous substrate according to the invention is considered to be made from a homogeneous cellulosic fibrous substrate. Without wishing to be bound by theory, it is believed that this effect is achieved due to the length of the cellulose fibers being below 10mm, preferably below 4 mm. As mentioned above, the short hydrophilic cellulose fibers are substantially completely impregnated with the binder. Further, when the stack of prepregs is subjected to high pressure and high temperature and formed into a cellulose fiber substrate, little cracks are formed because the cellulose fibers can be rearranged due to the short fiber length without breaking. The pressure may be at least 20kg/cm 2 Preferably at least 25kg/cm 2 More preferably 30kg/cm 2 And the temperature may be at least 60 ℃, preferably at least 140 ℃, more preferably at least 150 ℃. In particular, the temperature may be 148 ℃ to 152 ℃. Further, during the manufacturing process, even if a crack occurs in one layer of the stack of prepregs, it may be filled with cellulose fibers from at least one adjacent layer of the stack of prepregs.
When using a stack of prepregs, each layer of the stack of prepregs may be arranged relative to the other layers such that the longitudinal extension of the fibres is suitable for the intended use of the resulting cellulosic fibre substrate.
The thickness of each layer of the stack of prepregs may be from 0.01mm to 10mm. In fact, as described above, the thickness of each layer depends on the total thickness of the cellulosic fibrous substrate. Thus, if the cellulosic fibrous substrate comprises only one layer of cellulosic fibrous substrate, the thickness of the layer is substantially equal to the thickness of the cellulosic fibrous substrate. In the case where there are multiple layers, the thickness of each layer may be the same as or different from the thickness of the other layers in the stack of prepregs. The term "plurality" means at least two in the context of the present invention.
The stack of prepregs disclosed above may be a high pressure stack of prepregs (HPL). HPL is produced by impregnating a multi-ply kraft paper comprising cellulosic fibers with a binder.
The cellulosic fibrous substrate according to the present invention may comprise at least one surface layer. The term "surface layer" is in the context of the present invention understood to be a layer arranged on the surface of a cellulosic fibrous substrate. Such surface layers may be arranged so as to provide scratch resistance, UV resistance, food compatibility, aesthetic appearance, antimicrobial properties, color, surface structure, friction, or any other functionality that may be desired.
A method for manufacturing a cellulosic fibrous substrate by hot press molding may include the steps of:
a) Providing at least one sheet of cellulosic fibers having a maximum length of 10 mm;
b) Impregnating the at least one sheet of cellulose fibers with a mixture of an acid curing catalyst and a binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof;
c) Pre-curing the sheet of at least one impregnated cellulose fiber by heating in the range of 50 ℃ to 300 ℃ to obtain a prepreg;
d) Disposing one or more prepregs into a stack;
e) At least 7kg/cm in a pressing tool 2 Preferably at least 25kg/cm 2 More preferably at least 30kg/cm 2 Is pressed at a temperature of at least 60 ℃, preferably at least 140 ℃, more preferably at least 150 ℃A period of at least 10 seconds, preferably at least one minute, more preferably at least two minutes, to obtain a cellulosic fibrous substrate having at least a top surface and a bottom surface.
The above method may further comprise the step f) of edge cutting the cellulosic fibrous substrate and the step h) of creating cavities in the cellulosic fibrous substrate.
In summary, the present invention provides a cellulosic fibrous substrate comprising cellulosic fibers that are natural, readily available, highly recyclable, and thus environmentally friendly and cost effective materials. The unexpected and unexpected effect of the present invention is that the mechanical properties, such as bending and tensile strength, of the cellulosic fibrous substrates of the present invention are comparable to the tensile and/or bending strength of 3D articles made from GFRP, but made from a combination of short cellulosic fibers and a bio-based binder, which provides design freedom to create complex 3D surfaces that contain, inter alia, non-deployable portions. Another advantage of the present invention is the use of by-products from the food and agricultural industries as binders, which contributes to recycling economy and is environmentally beneficial.
While the invention has been illustrated in the drawings and foregoing description, such illustration is to be considered illustrative or exemplary and not restrictive; the invention is not limited to the disclosed embodiments. Other variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed invention, from a study of the drawings, the disclosure, and the appended claims. In the appended claims, the word "comprising" does not exclude other elements or steps, and the indefinite article "a" or "an" does not exclude a plurality. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage. Any reference signs in the claims shall not be construed as limiting the scope.
Claims (22)
1. A cellulosic fibrous substrate comprising:
at least one of the top surfaces of the base plate,
at least one of the bottom surfaces of the base plate,
characterized in that the cellulosic fibrous substrate further comprises:
60 to 90wt% of cellulose fibers having a length of at most 10mm,
0 to 10% of an acidic curing catalyst
10 to 40wt% of a binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof.
2. The cellulosic fibrous substrate of claim 1 wherein the binder is polyfurfuryl alcohol (PFA).
3. The cellulosic fibrous substrate of any of the preceding claims, wherein the cellulosic fibers comprise 0-100% virgin cellulosic fibers and 0-100% recycled cellulosic fibers.
4. A cellulosic fibrous substrate according to any of the preceding claims, wherein the at least one top and/or bottom surface has at least one expandable and/or non-expandable surface portion.
5. The cellulosic fibrous substrate of any of the preceding claims, wherein the cellulosic fibers are arranged substantially parallel in the substrate, or wherein the cellulosic fibers are arranged substantially cross-wise in the substrate, or wherein the cellulosic fibers are arranged substantially randomly or in a combination thereof in the substrate.
6. A cellulosic fibrous substrate as claimed in any preceding claim, wherein the substrate comprises at least one cavity.
7. A load bearing 3D article comprising the cellulosic fibrous substrate according to any of the preceding claims.
8. The load bearing 3D article of claim 10, wherein the load bearing article has a tensile strength of at least 40MPa, preferably at least 50MPa, more preferably at least 100 MPa.
9. The carrier 3D article of claim 10 or 8, wherein the carrier article has a thickness of at least 2.5mm, preferably at least 5mm, more preferably at least 10mm.
10. A method for manufacturing a cellulosic fibrous substrate comprising at least a top surface and a bottom surface, the method comprising the steps of:
a) Providing at least one sheet of cellulosic fibers having a maximum length of 10 mm;
b) Impregnating the at least one sheet of cellulose fibers with a mixture of an acid curing catalyst and a binder selected from the group consisting of: cellulose, hemicellulose, furan, lignin, and combinations thereof;
c) Pre-curing the sheet of at least one impregnated cellulose fiber by heating in the range of 50 ℃ to 300 ℃ to obtain a prepreg;
d) Disposing one or more prepregs into a stack;
e) At least 7kg/cm in a pressing tool 2 Preferably at least 25kg/cm 2 More preferably at least 30kg/cm 2 And a temperature of at least 60 ℃, preferably at least 140 ℃, more preferably at least 150 ℃ for a period of at least 10 seconds, preferably at least one minute, more preferably at least two minutes, to obtain a cellulosic fibrous substrate having at least one top surface and one bottom surface.
11. The method for manufacturing a cellulosic fibrous substrate according to claim 10, wherein the binder is polyfurfuryl alcohol (PFA).
12. The method for manufacturing a cellulosic fibrous substrate according to claim 10 or 11, wherein the cellulosic fibers comprise a mixture of 0-100% virgin cellulosic fibers and 0-100% recycled cellulosic fibers.
13. The method for manufacturing a cellulosic fibrous substrate according to claims 10-12, wherein the cellulosic fibers are provided in the form of paper.
14. The method for manufacturing a cellulosic fibrous substrate according to claims 10-13, wherein the top and/or bottom surface has at least one expandable and/or non-expandable surface portion.
15. The method for manufacturing a cellulosic fibrous substrate according to claims 10-14, wherein the cellulosic fibrous substrate has a biobased carbon in an amount of at least 80%.
16. The method for manufacturing a cellulosic fibrous substrate according to claims 10-15, wherein the cellulosic fibrous substrate comprises 60 to 90wt% of the cellulosic fibers.
17. The method for manufacturing a cellulosic fibrous substrate according to claims 10-16, wherein the cellulosic fibrous substrate comprises 10 to 40wt% of the binder.
18. The method for manufacturing a cellulosic fibrous substrate according to claims 10-17, wherein the cellulosic fibrous substrate comprises 0 to 10wt% of the acidic catalyst.
19. A method for manufacturing a cellulosic fibrous substrate according to claims 10-18, wherein the prepregs in the stack are oriented such that the directions of the textures in the prepregs are substantially parallel.
20. A method for manufacturing a cellulosic fibrous substrate according to claims 10-19, wherein the prepregs in the stack are oriented such that the angle of the grain direction in the prepregs is in the range of 0-90 ° relative to the adjacent prepregs.
21. The method for manufacturing a cellulosic fibrous substrate according to claims 10-20, further comprising the step f) of cutting the prepreg and/or the cellulosic fibrous substrate into a predetermined shape.
22. The method for manufacturing a cellulosic fibrous substrate according to claims 10-21, further comprising step g) of creating cavities in the cellulosic fibrous substrate.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP21184323.0 | 2021-07-07 | ||
| SE2151397-3 | 2021-11-16 | ||
| SE2151397A SE2151397A1 (en) | 2021-07-07 | 2021-11-16 | A 3d article comprising cellulosic fibers and having improved strength |
| PCT/EP2022/068740 WO2023280918A1 (en) | 2021-07-07 | 2022-07-06 | Cellulosic fiber material and process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117580896A true CN117580896A (en) | 2024-02-20 |
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| CN202280046194.1A Pending CN117580896A (en) | 2021-07-07 | 2022-07-06 | Cellulosic fibrous material and method |
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