EP4036306A1 - Produit de réseau tridimensionnel de fibres biodégradables à partir de fibres organiques naturelles, son procédé de préparation et d'utilisation - Google Patents

Produit de réseau tridimensionnel de fibres biodégradables à partir de fibres organiques naturelles, son procédé de préparation et d'utilisation Download PDF

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Publication number
EP4036306A1
EP4036306A1 EP21154700.5A EP21154700A EP4036306A1 EP 4036306 A1 EP4036306 A1 EP 4036306A1 EP 21154700 A EP21154700 A EP 21154700A EP 4036306 A1 EP4036306 A1 EP 4036306A1
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Prior art keywords
natural organic
fibre network
network product
organic fibres
fibres
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EP21154700.5A
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German (de)
English (en)
Inventor
Rafal Brzyski
Michal Ziólkowski
Mateusz Szafranski
Andrii Holovin
Monika Jezak
Jakub Sosinski
Pawel Przybyszewski
Tomasz CIAMULSKI
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Organic Disposables Sp zoo
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Organic Disposables Sp zoo
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Priority to EP21154700.5A priority Critical patent/EP4036306A1/fr
Priority to EP22154829.0A priority patent/EP4036307A1/fr
Publication of EP4036306A1 publication Critical patent/EP4036306A1/fr
Withdrawn legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21J—FIBREBOARD; MANUFACTURE OF ARTICLES FROM CELLULOSIC FIBROUS SUSPENSIONS OR FROM PAPIER-MACHE
    • D21J3/00—Manufacture of articles by pressing wet fibre pulp, or papier-mâché, between moulds

Definitions

  • the present invention relates to a biodegradable three-dimensional fibre network product from defibrated natural organic fibres, method of preparation of the fibre network product using electromagnetic (EM) energy and use thereof.
  • EM electromagnetic
  • Natural organic fibres of plants or animal origin have been widely used for many years in many industries, such as paper and wood industry, due to advantageous mechanical properties including good tensile strength, low weight and specific stiffness, but also due to its renewable character and ability to be broken down by bacteria making them environment friendly.
  • cellulose fibres used as raw material are wetted, converted into a pulp, pressed, and dried giving sheets of paper having a substantially flat shape, wherein the fibres are oriented substantially in the sheet-plane direction, which results in a product having a good tensile strength in said sheet-plane direction. Compression into thin sheets of paper allows for effective removal of water from the material, whereas production of thicker sheets is limited and requires more energy to dry the final product.
  • Timofeev, et al. "Drying of foam-formed mats from virgin pine fibers", (2016), Drying Technology, 34:10, 1210-1218 , describes drying of foam-formed mats from virgin pine fibres using the steps of fibre foam preparation, draining of the liquid, and drying with the use of different drying methods, namely convective drying in the oven, impingement drying assisted by vacuum, combined impingement-infrared drying, and through-air drying. Shrinkage of the final product was observed in all tested drying methods with the lowest shrinkage observed for combined techniques.
  • Wood fibres are widely used for the manufacturing of fibreboards (such as MDF or HDF), however, in order to obtain desired properties of the fibreboard, fibres are mixed with a synthetic binder and formed into panels by hot-pressing. Synthetic binders used in the production of fibreboards are not environmentally friendly and such materials have limited uses.
  • An aspect of the present invention is to provide a method for the preparation of a three-dimensional biodegradable fibre network product using electromagnetic energy.
  • the method allows to control density and anisotropy inside the product and forming it into any shape.
  • the method has very short forming times of the product.
  • Another aspect of the present invention is to provide a three-dimensional biodegradable fibre network product as defined by claim 12.
  • Preferable embodiments of the product according to this aspect are defined in dependent claims.
  • the product having good mechanical strength and stability is provided.
  • the product has high over 95% porosity and low material density down to 8 kg/m 3 .
  • Another aspect of the present invention is to provide a use of said product as defined in claim 15.
  • references in the specification to "an embodiment”, “one embodiment”, “another embodiment”, etc., indicate that the embodiment described may include one or more features. Additionally, when features are described in connection with one embodiment, it should be understood that such features may also be used in connection with other embodiments whether or not explicitly described unless clearly stated to the contrary.
  • the present invention provides a method for the preparation of a three-dimensional biodegradable fibre network product, the method comprising:
  • the method according to the present invention allows for controlling of density gradient of the three-dimensional biodegradable fibre network product in any direction in the whole space of the mould.
  • Density gradient of the three-dimensional biodegradable fibre network product prepared by the method according to the present invention is controlled by the arrangement of the plurality of pores in a mould. Density gradient of the three-dimensional biodegradable fibre network product prepared by the method according to the present invention is also controlled by the kind and/or power density of electromagnetic energy provided to the foamed natural organic fibres. Preferably, density gradient of the three-dimensional biodegradable fibre network product prepared by the method according to the present invention is controlled by the arrangement of the plurality of pores in a mould and by the kind and/or power density of electromagnetic energy provided to the foamed natural organic fibres. Mould with fewer pores having foamed fibres subjected to electromagnetic energy with higher power densities of electromagnetic energy results in obtaining higher density gradient in the three-dimensional biodegradable fibre network product.
  • the density of the fibre network product prepared by the method according to the present invention is also controlled by the density of the foam. Lowering foam density, leads to a fibre network product with lower density, and with higher density gradient.
  • Providing electromagnetic energy to the foamed natural organic fibres in a mould with a plurality of pores results in volumetric heating of the foamed natural organic fibres, that leads to the generation of steam and increase in pressure. This results in reorientation of the fibres in certain direction from the inside of the mould.
  • These directions are controlled by the arrangement of the pores adapted to evacuate water and steam.
  • the arrangement of the pores comprises pore size, pore shape, pore direction, number of pores in the mould, distance from the pores.
  • the arrangement of the pores sets direction of the steam release path causing compaction of the fibres at the walls of the mould, leading to reinforcement of the final fibre network product. Density gradient of the fibre network product is therefore controlled in a wide range.
  • the method provides a three-dimensional biodegradable fibre network product, which is empty inside. Also, the density of the structure is controlled by the amount of natural organic fibres put into the mould.
  • Providing electromagnetic energy comprises one or more phases, preferably an initial phase and a final phase.
  • electromagnetic energy is delivered intensively to reach water boiling point, which results in forcing the excess of water out of the mould.
  • This initial phase saves energy and time required to evaporate the remaining water, which should be removed and preserves the fibrous web/mesh structure from collapsing/shrinking inside the mould.
  • bonds between natural organic fibres are created forming fibre network product.
  • different electromagnetic energy levels can be required in consecutive phases, for instance, in order to prevent local overheating of the material.
  • pure cellulose fibres as well as ligno-cellulose fibres that have been defibrated mechanically can be used as natural organic fibres for the present invention.
  • Cellulose fibres similar to those used in paper production (after removing the lignin), plant fibres, and other organic fibres, multiversity of which is expected due to their nature can be used.
  • ligno-cellulose fibres that are fractioned mechanically (without removing the lignin) are suitable.
  • Natural organic fibres of one type or as mixture of different type of fibres can be used with the present invention (e.g., by weight: 50% cellulose fibres, 50% hemp fibres - a composition that is more crack resistant than 100% cellulose). Crack resistance is achieved by incorporating long (up to 30mm) natural fibres into the foam. The likely mechanism is that there is an increase in the interaction between a greater number of fibres per volume of the product.
  • the content of natural organic fibres in three-dimensional fibre network product is at least 95% on a dry basis.
  • the length of natural organic fibres is from 0.1 cm to 3.0 cm.
  • natural organic fibres are cellulose fibres.
  • natural organic fibres are ligno-cellulose fibres.
  • natural organic fibres are a combination of cellulose fibres and ligno-cellulose fibres.
  • foaming natural organic fibres is performed in aqueous solution.
  • the parameters of the foam, and particularly the degree of foaming, have a significant effect on the internal structure of the final fibre network product prepared by the method of the present invention.
  • Foam is a good dispersing medium for fibres in the three-dimensional network and any suitable method of foaming known in the prior art can be used for the method according to the present invention.
  • the size of the foam bubbles determines the distribution of fibres in the three-dimensional space. Therefore, controlling the bubbles allow for obtaining a controlled density gradient in the fibre network product prepared by the method of the present invention.
  • foaming natural organic fibres in aqueous solution is performed by introducing a gas into the pulp.
  • the size and homogeneity of the foam bubbles are influenced by the different phases of the forming process.
  • the stage of preparing the batch of material gives the possibility of shaping the character of the foam by adding to the mass some additives: blowing agents increase the amount of the gas filling the bubbles, surfactants control the foam's susceptibility to foaming.
  • blowing agents increase the amount of the gas filling the bubbles
  • surfactants control the foam's susceptibility to foaming.
  • foam stabilizers allows the foam to maintain the desired properties until the fibres stiffen and take over the role of a supporting skeleton a structure that has so far been held by vanishing bubbles.
  • aqueous solution used for foaming natural organic fibres further comprises at least one biodegradable non-fibrous additive comprising a foam stabilizer, foaming agent, biodegradable blowing agent or combination thereof.
  • Biodegradable foam stabilizers in form of polysaccharides can be used with the method of the present invention.
  • chitosan and/or agar are preferable biodegradable foam stabilizers.
  • Their main goal of foam stabilizers is to extend the life of wet foam, and to support the mechanical stability of the final product.
  • Biodegradable foaming agents meeting environmental standards can be used with the method of the present invention.
  • coco glucoside is a preferred foaming agent.
  • Biodegradable blowing agents introduced into the water solution can also be used as an aid in the formation of foam.
  • the preferred blowing agents are sodium carbonate and sodium bicarbonate, which have minimal impact on the environment.
  • aqueous solution used for foaming natural organic fibres further comprises at least one further additive for controlling biomechanical properties of the obtained fibre network product, wherein said further additive comprise a polysaccharide, polysaccharide derivative, lignin, lignin derivative, cellulose, and a cellulose derivative.
  • non-fibrous additives can be used with the method of the present invention to define end parameters of the material.
  • Some of the additives have a double role, as a material stabilizer and foam enhancers.
  • biomaterials that are at least partially dissolvable in water are used.
  • Preferred non-fibrous additives are agar and chitosan, polysaccharides, that are helping with moisture control and stiffness of the product.
  • Agar gel acts as a foam stabilizer, that extends the life of wet foam, and after electromagnetic forming it acts as a gluing agent, improving the strength of bonds between fibres.
  • Hydrophilic additives e.g., chitosan
  • Hydrophilic additives can be added for agricultural uses of the product obtained by the method according to the present invention, for maintaining moisture for a prolonged time.
  • Biological additives e.g., grapefruit extract
  • Water insoluble, hydrophobic additives e.g., mineral powders
  • mineral powders can be added for creating solutions for construction applications for water repellence.
  • polysaccharides are used as a foam additive to increase the durability of the fibre network product after the forming process.
  • the suitable polysaccharides comprise agarose, chitosan and combination thereof. Agarose mechanically stabilizes the material after forming, by strengthening the bonds between the fibres and securing their surface mechanically. Chitosan, in addition to performing the function of mechanical strengthening, is known for its biocidal properties, protects the material against excessive biological aging.
  • starch is also used as a foam additive, which increases the stiffness of the material after the molding process.
  • Starch is a potential additive, that has impact on mechanical properties of the final material. It makes the outer layer more rigid and brittle.
  • lignin is used as an additive. Lignin may be introduced to increase mechanical strength and water resistance of final product.
  • chemical and mechanical derivatives of cellulose can be used as mechanical stabilizers or modifiers of the fibre surface.
  • examples include cellulose ethers, for example, methyl cellulose and ethyl cellulose, known for their use as industrial rheology modifiers. They can be used as foam stabilizing agents and modifier of interactions between the fibre network product and solvents, either polar or nonpolar.
  • Other cellulose derivatives including hydroxypropylmethylcellulose and cellulose nanofibrils are suitable additives using the method according with the present invention.
  • Fig. 1 the method of the present invention is illustrated, wherein in the initial fibres preparation step, stock natural organic fibres, such as cellulose fibres are being defibrated using already known methods.
  • the obtained defibrated natural organic fibres are suspended in water to obtain an aqueous solution.
  • aggregation and foaming of the natural organic fibres in aqueous solution is performed.
  • foam creation There are many methods supporting the foam creation during this phase. It could be done by injecting a gas through nozzles, shaking/ultrasounds, mechanical mixing or increasing the gas saturation by increasing the pressure in the mixing chamber (generating overpressure relative to the forming process pressure).
  • additional additives can be added.
  • mould filing is performed and foamed natural organic fibres are placed in a mould of arbitrary size and shape.
  • Three-dimensional mould is used to control the of shape the fibre network product as well as to limit the foamed material expansion during the fast thermodynamical process (scaling of production speed).
  • the mould has a plurality of pores to allow for evaporation of steam and gases during forming. The number of pores and its size allows for control of the density gradient and other physical characteristics of the fibre network product obtained in the method according to the present invention. Pores can be small, but also can have a form of missed walls or parts of the walls of the mould.
  • the mould is made of material, having a softening point above 100°C. In one embodiment the mould is at least partially made of a dielectric material selected from PVC, PVL, silicon, PTFE, PTFE GF30, PP-H, PEEK, ceramics, or combination thereof.
  • EM material forming is performed as depicted in Fig. 1 .
  • electromagnetic energy is provided to the foamed natural organic fibres in the mould.
  • kind of electromagnetic energy in terms of frequency and power density is adapted to desired properties of the final fibre network product prepared.
  • electromagnetic energy having a frequency in a range of 10 - 100 MHz is provided to the foamed natural organic fibres.
  • This frequency range is preferable for implementation of electromagnetic energy delivery device in a form of parallel plate capacitor or almost parallel plate capacitor. Relation of wavelength to the device size allows for such implementation. Such implementation allows for automation of the material forming in continuous process, while the material is moving along parallel plates.
  • the capacitor is popular implementation in the industry around 27 - 35 MHz frequency range. Another advantage of this frequency range is that electromagnetic energy can be better dissipated in losses in natural organic fibrous material and polymer additives.
  • electromagnetic energy having a frequency in a range of 300 MHz - 10 GHz is provided to the foamed natural organic fibres.
  • This frequency range is preferable for implementation of electromagnetic energy delivery device in a form of a resonator, usually built as a closed cavity or a tunnel with the resonance inside the tunnel.
  • Another advantage of this frequency range is that electromagnetic energy can be better dissipated in water, especially at 2.4 GHz resonance of water particles.
  • the tunnel resonances are popular implementation in the industry around 900 MHz frequency.
  • electromagnetic energy is provided uniformly. This can be achieved by a combination of uniform electromagnetic field generation technique and physical movement (longitudinal or rotations) of the mould within the semi-uniform electromagnetic field.
  • a ventilation system is used, allowing for removal of moisture from the space surrounding the form.
  • the efficiency of the ventilation increases for shorter forming times (higher powers of electromagnetic energy can be applied).
  • the delivery of warm air can further optimize the forming process in combination with the delivery of electromagnetic energy.
  • mould may be optionally unpacked and further drying of the obtained fibre network product can be done by applying a flow of dry air and conventional heating (with or without applying of electromagnetic energy). This optional step is marked as auxiliary drying on Fig. 1 .
  • Fig. 2 the shape of a closed mould according to an embodiment is illustrated.
  • Three of the four walls are flat and perpendicular to each other, the fourth is spherical. All of the outer surfaces have different normal vectors.
  • On the two flat walls and the spherical one there are pores in a form of round holes drilled through the walls. Diameters of those holes and distribution density are varied.
  • Fig. 3 the interior of a mould from Fig. 2 is illustrated for better understanding of the invention.
  • the walls of the mould limit and determine the shape of the formed material. They are themselves impermeable to water vapor, but thanks to the holes, water vapor escapes through three of the four walls of the mould.
  • Fig. 4 shows a cross section of the mould according to an embodiment (the same as shown in Fig. 3 and Fig. 4 ) with an indication of pressure gradients depending on mould shape and pore placements.
  • the temperature of the foamy material inside the mould increases simultaneously throughout the entire volume of the mould. It is because EM energy is accumulated over the entire volume of foamy material, i.e. by all the mass contained in the mould.
  • the temperature reaches the boiling point of water, an intense process of water vapor formation begins, the more intense the higher the power density used in the process. This creates a pressure build-up that seeks to escape through the pores in the mould walls.
  • the lines of the steam flow currents are shaped by pressure gradients, and those in the area of the pores coincide with the vectors normal to the wall surfaces in these places. Those lines of steam flow generate pressure on fibres, which are wet in the first phase of the process and susceptible to displacement and crushing. That is why the density of the final fibre network product may be non-uniform. Moreover, we can distinguish many directions along which the density increases. These density gradients coincide with the pressure gradients shown in Fig. 4 .
  • the steam leakage rate also depends on the size of individual pores, their shape, and the density of their distribution. As illustrated in Fig. 4 , more steam will flow through the area of the pores on the spherical wall at the same time than through the remaining open areas of the mould. This is due to the much larger diameter of the pores on the spherical wall and a relatively large number of them.
  • the density distribution in the product obtained from such mould has a smaller material density gradient from the spherical side, but it remains much more even over a large area - similar to the pressure gradient distribution shown in Fig. 4 .
  • Fragments of a final fibre network product obtained according to an embodiment, which was located adjacent to the flat walls in the regions corresponding to the pores in the mould have a greater density of the material, the fibre network product is strengthened, but only in a small area covered by the "action" of the mould pores. It is significant that from the side of the third flat wall, which is adjacent to the solid wall (without pores) of the mould, it is more difficult to distinguish a clear differentiation of density, the density gradient is absent, and the obtained fibre network product is softer.
  • pores in bottom part of the mould could normally serve as drainage holes for water excess removal by gravitation or by additional application of vacuum.
  • such process usually leads to some degradation of the foam.
  • the draining step is not used and excess of water is forced out of the mould by application of electromagnetic energy at a level which causes water boiling inside the mould.
  • parts of the mould are composed of metal parts of the electromagnetic field delivery device.
  • parallel metal plates of a capacitor can also serve as upper or lower walls of the mould allowing to form larger sheets of material.
  • parts of the mould or electromagnetic field delivery device have movable elements which allow automatizing the manufacturing process of material filling into the mould, travelling through the mould or removing it out of the mould after the formation of the final fibre network product.
  • a three-dimensional biodegradable fibre network product is provided, wherein the fibre network product is prepared from foamed natural organic fibres using electromagnetic energy, wherein the fibre network product has a density of 8 - 150 kg/m 3 and total porosity of more than 90%.
  • the product has a density of 8 - 90 kg/m 3 , preferably a density of 8 - 70 kg/m 3 , more preferably a density of 8 - 50 kg/m 3 , the most preferably a density of 8 - 30 kg/m 3 .
  • the physical properties of the structure according to the invention can be determined by the method described by the Research Station in Naaldwijk, Netherlands (Wever '2002). Used standards: PN-EN 13039 - determination of organic matter content, PN-EN 13041 - determination of total porosity, volume density, shrinkage, water and air capacity at a water potential of -10 cm H 2 O.
  • a fibre network product prepared by the method of the present invention having the following characteristics:
  • Fig. 5 shows water retention curve for the fibre network product according to an embodiment of the present invention.
  • the X-axis represents a potential from 0 to -10 cm H 2 O
  • the Y-axis represents water volume (vol %).
  • the fibre network product according to the embodiment of the present invention is characterized by high water and air capacity of more than 45%, which favours the growth of young plants such as seedlings.
  • the tested fibre network product in a form of cubes also have an appropriate pH of 6 - 7 and are characterized by a very low EC, which greatly facilitates the selection of optimal fertilization.
  • the preferred density of the fibre network product is about 70 kg/m 3 (in the range of 65 - 75 kg/m 3 ).
  • the fibre network product with such a density has the most advantageous air-water properties, similar to those of mineral wool.
  • Fig. 6 illustrates different embodiments a), b), c) and d) of a mould integration with electromagnetic field delivery device, cross-sectional view:
  • the three-dimensional biodegradable fibre network product of the present invention can be preferably used as a plant growth substrate, filtration medium, filling and/or acoustic and mechanical damping structure.
  • the product was prepared according to the following steps:
  • the method presented in example 1 makes it possible to obtain structures with high mechanical strength and high impact strength in relation to their mass.
  • the product was prepared according to the following steps:
  • the product was prepared according to the following steps:
  • the method provided in example 3 allows to obtain a material with good water absorption and favourable air-water relation for plant growth.

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  • Manufacturing & Machinery (AREA)
  • Nonwoven Fabrics (AREA)
EP21154700.5A 2021-02-02 2021-02-02 Produit de réseau tridimensionnel de fibres biodégradables à partir de fibres organiques naturelles, son procédé de préparation et d'utilisation Withdrawn EP4036306A1 (fr)

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Application Number Priority Date Filing Date Title
EP21154700.5A EP4036306A1 (fr) 2021-02-02 2021-02-02 Produit de réseau tridimensionnel de fibres biodégradables à partir de fibres organiques naturelles, son procédé de préparation et d'utilisation
EP22154829.0A EP4036307A1 (fr) 2021-02-02 2022-02-02 Appareil et procédé de préparation d'un produit de réseau de fibres biodégradables tridimensionnel de fibres organiques naturelles, ledit produit et son utilisation

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EP21154700.5A EP4036306A1 (fr) 2021-02-02 2021-02-02 Produit de réseau tridimensionnel de fibres biodégradables à partir de fibres organiques naturelles, son procédé de préparation et d'utilisation

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EP22154829.0A Pending EP4036307A1 (fr) 2021-02-02 2022-02-02 Appareil et procédé de préparation d'un produit de réseau de fibres biodégradables tridimensionnel de fibres organiques naturelles, ledit produit et son utilisation

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Cited By (1)

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US20230074870A1 (en) * 2019-12-31 2023-03-09 Kimberly-Clark Worldwide, Inc. Foam-based manufacturing system and process

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WO2024051915A1 (fr) * 2022-09-05 2024-03-14 Storopack Hans Reichenecker Gmbh Procédé permettant de fabriquer un article composé au moins en partie de fibres de cellulose, et article composé au moins en partie de fibres de cellulose

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WO2018237279A1 (fr) * 2017-06-22 2018-12-27 Materialise Nv Structures perforées

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US20010024716A1 (en) * 1998-05-22 2001-09-27 Fung-Jou Chen Fibrous absorbent material and methods of making the same
WO2018237279A1 (fr) * 2017-06-22 2018-12-27 Materialise Nv Structures perforées

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ALIMADADI ET AL.: "3D-oriented fiber networks made by foam forming", CELLULOSE, vol. 23, 2016, pages 661 - 671, XP035903987, DOI: 10.1007/s10570-015-0811-z
BURKE ET AL.: "Properties of lightweight fibrous structures made by a novel foam-forming technique", CELLULOSE, vol. 26, 2019, pages 2529 - 2539, XP036728885, DOI: 10.1007/s10570-018-2205-5
TIMOFEEV ET AL.: "Drying of foam-formed mats from virgin pine fibers", DRYING TECHNOLOGY, vol. 34, no. 10, 2016, pages 1210 - 1218

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20230074870A1 (en) * 2019-12-31 2023-03-09 Kimberly-Clark Worldwide, Inc. Foam-based manufacturing system and process
US11932988B2 (en) * 2019-12-31 2024-03-19 Kimberly-Clark Worldwide, Inc. Foam-based manufacturing system and process

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