• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a method for manufacturing a part from a natural material in particulate form containing scleroproteins. This method comprises a heating phase of the material under compression at a pressure greater than or equal to 30 MPa, at a temperature greater than or equal to the denaturation temperature of the scleroproteins contained in the material. It then comprises a cooling phase of the material thus obtained to a temperature below 100 ° C, maintaining the compression during at least part of the cooling phase.
    公开号:FR3072680A1
    申请号:FR1759886
    申请日:2017-10-20
    公开日:2019-04-26
    发明作者:Vincent Menny；Antoine Rouilly；Alain Couret；Dimitri Mazars；David Neumeyer；Virginie VANDENBOSSCHE；Jean Monchoux；Foad Naimi
    申请人:Authentic Mat；Toulouse Tech Transfer；Centre National de la Recherche Scientifique CNRS；Institut National Polytechnique de Toulouse INPT；Institut National de la Recherche Agronomique INRA；
    IPC主号:
    专利说明:

    The present invention is in the field of the recovery of protein residues of animal origin.
    More particularly, the present invention relates to a method of manufacturing a part from a natural material in particulate form containing scleroproteins. The invention also relates to a part obtained by such a manufacturing process, and the use of such a part for the manufacture of an eyewear, jewelry or tableware item.
    The planned depletion of fossil resources has for several years been encouraging manufacturers to develop alternative solutions using renewable resources, and this in all areas of industry. The recycling and recovery of animal or vegetable waste is of increasing interest in this respect, both from an economic and environmental point of view.
    It has thus been proposed in the prior art to manufacture solid materials from animal or vegetable waste, in particular by a hot and high pressure molding process for this waste.
    An example of such a process is described in document WO 2012/069736, for the manufacture of a solid material from an organic material of plant origin containing polysaccharides or polypeptides.
    The present inventors are more particularly interested in natural raw materials of non-human animal origin, and in particular based on a particular type of protein, scleroproteins.
    Scleroproteins, otherwise known as fibrous proteins, constitute one of the three main classes of animal proteins. These are long molecules in the form of filaments, playing a structural and constitutive role in the body, and used in the composition of so-called support tissues, such as bones and connective tissues, as well as integuments, such as skin, hair, horns, hooves and nails. There are different types: keratins, which form protective tissues in the body, such as the epidermis, hair, nails, hooves, horns or feathers of birds; collagens, which are connective tissues, such as cartilage; conchyoline, which forms the shells of molluscs; and elastins, also found in connective tissues.
    Many industrial wastes from animal husbandry, such as horn, feathers, leather, or production waste, such as scrap generated during leather work or horn work, etc., mainly consist of scleroproteins. The use of this waste for the manufacture of parts in solid material, intended for multiple and varied applications taking advantage of the aesthetic and mechanical properties of these natural materials, would allow a quite interesting recovery, economically and environmentally.
    At the origin of the present invention, it was discovered by the present inventors that a process for treatment by compression at high temperature of natural materials in particulate form based on scleroproteins, such as materials based on leather or horn animal, for example, this process being implemented under specific operating conditions, makes it possible to form massive parts of a material having particularly advantageous mechanical properties, in particular good cohesion, homogeneous structure, good physical and aesthetic stability, and with a low degree of hygroscopy.
    Thus, the present invention aims to propose a method of manufacturing a part from a natural material in particulate form based on scleroproteins, which makes it possible to obtain a solid material reproducing the properties of the initial natural material, and even improving some of these properties.
    An additional objective of the invention is that this process is simple and quick to implement.
    In the present description, the term “natural material” means a material of natural origin, as opposed to synthetic materials, such as a material of animal origin.
    In order to achieve the above objectives, there is proposed according to the present invention a method of manufacturing a part from a natural material in particulate form containing scleroproteins. This process includes:
    a phase of heating said natural material under compression at a pressure greater than or equal to 30 MPa, at a temperature greater than or equal to the denaturation temperature of the scleroproteins entering into the composition of this material,
    - And a cooling phase of the material thus obtained, called denatured material, to a temperature below 100 ° C.
    The compression is maintained during at least part of this cooling phase, preferably during at least the initial part of this cooling phase.
    Preferably, the compression is maintained throughout the cooling phase.
    Typically, the material to which the process according to the invention is applied, of natural origin, contains more than 50% by weight of scleroproteins, scleroproteins being substantially the only type of proteins present therein.
    It is within the competence of a person skilled in the art to determine, for a given initial natural material, what is the denaturing temperature of the scleroproteins which enter into its constitution, under the pressure conditions applied in the device used. This temperature depends in particular on the moisture content of the material. To this end, the person skilled in the art may in particular carry out an analysis of the initial material by a technique known per se for the measurement of this parameter, for example by the differential scanning calorimetry (DSC) technique, according to a mode classic operating room. Knowing the moisture content of the material on which he wishes to implement the method according to the invention, the person skilled in the art may otherwise refer, in order to know the denaturation temperature of the scleroproteins, to a preset chart, in particular by analyzes by DSC of samples of this material with different humidity levels, such as the chart shown in Figure 1 attached.
    Heating the natural material to a temperature greater than or equal to the denaturation temperature of the scleroproteins causes a phase change in the organized zones of these proteins, in particular the zones with a helix structure (s) and / or sheet (s). β, and a loss of structure in these organized areas. The deformability of the material increases accordingly. In doing so, the compression exerted on the material in accordance with the invention advantageously makes it possible to prevent water from accumulating in the pores of the material.
    The heating phase is also advantageously carried out at a temperature which remains below the degradation temperature of the scleroproteins. It is within the skill of a person skilled in the art to know how to determine this degradation temperature. To this end, it may in particular carry out a thermogravimetric analysis (ATG) of a sample of the natural material, in a conventional manner in itself.
    The so-called denatured material obtained at the end of the heating phase is then cooled, still under compression, to a temperature below 100 ° C., ensuring that the denatured material no longer contains water in the gaseous state.
    Preferably, the denatured material is cooled to a temperature below its glass transition temperature. This glass transition temperature can easily be determined by a person skilled in the art, using any technique known for this purpose, for example by dynamic mechanical analysis (DMA), carried out on a sample of the denatured material.
    Below its glass transition temperature, the material obtained returns, in a conventional manner in itself, to the glassy, non-deformable state. The release of the part produced by the process according to the invention is then advantageously facilitated.
    Preferably, the cooling phase is carried out as quickly as possible, as a function of what the apparatus used for implementing the method according to the invention allows.
    The process according to the present invention is carried out dry, on the initial natural material in the solid state. It advantageously does not use any solvent.
    At the end of the process according to the invention, a part is formed from a block of solid material having the aesthetic appearance of the natural starting material, and having good cohesion and good solidity, of homogeneous structure, physically and aesthetically. stable. This material also has a lower hygroscopy, and a higher density, than that of the natural starting material. This densification gives the material of the part obtained improved mechanical properties, in particular good mechanical resistance and low deformability, as well as better resistance to humidity than the initial natural material. The part obtained also has a flexural modulus and a tensile modulus similar to, or even better than, those of the initial natural material.
    The method according to the invention, simple and quick to implement, also makes it possible to control the properties of the final material, in particular by adding suitable additives to the initial natural material upstream of the heating phase.
    It also makes it possible to perfectly control the shape and dimensions of the part formed, so that it is possible to manufacture parts suitable for all the desired applications.
    To this end, the method according to the invention can be implemented by compression of the initial material in particulate form contained in a mold of suitable shape and dimensions and implementation of the heating phase, then of the cooling phase, on the material in this mold.
    Such a mold is classic in itself. It can for example be formed from steel, graphite, tungsten carbide or silicone.
    Otherwise, the method according to the invention may comprise a prior step of cold preforming the natural material in particulate form, to form a solid preform which is then subjected to the heating phase, then to the cooling phase, under compression, of the method according to the invention.
    The method according to the invention can also respond to one or more of the characteristics described below, implemented in isolation or in each of their technically operating combinations.
    In particular embodiments of the invention, the heating phase of the natural material is carried out by flash sintering. The cooling phase is carried out in the same flash sintering device, without any intermediate manipulation of the material contained therein.
    The flash sintering technique (known as SPS, for Spark Plasma Sintering) is well known to those skilled in the art. It consists in passing a pulsed electric current through a matrix of electrically conductive material, containing the pulverulent material compacted in a uniaxial direction. This causes the material to heat by Joule effect and electrical and thermal conduction.
    In the context of the method according to the invention, this technique can be implemented in a conventional flash sintering device in itself, and according to operating conditions which are also conventional in themselves. The tools used may for example consist of graphite dies and pistons, but any other electrically conductive material, in particular steel, is also suitable.
    The implementation according to the invention of the flash sintering technique makes it possible to obtain a particularly dense final material, of particularly homogeneous structure and having particularly good mechanical properties.
    Otherwise, the heating step of the process according to the invention can be carried out by the technique, also conventional in itself, of hot pressing, or high pressure thermomolding.
    The process according to the invention can be carried out at atmospheric pressure, or at reduced pressure.
    Preferably, the gases released from the natural material during the heating phase are continuously removed from the device used. Thus, the process according to the invention preferably comprises, during the heating phase, and preferably also during the cooling phase, a step of continuous degassing of the enclosure containing the natural material on which the process is implemented.
    Prior to the heating step, the method according to the invention may comprise steps of cleaning, sorting and / or degreasing of the natural material, as well as, where appropriate, a prior step of grinding this natural material so as to ensure that it is in a particulate form, and if necessary at the desired particle size.
    Preferably, the particles of natural material in particulate form containing scleroproteins, on which the process according to the invention is applied, all have a diameter between 20 and 500 μιτι, preferably between 100 and 500 μιτι.
    Preferably, these particles have good size homogeneity.
    These particles also preferably have good shape homogeneity, which can in particular be ascertained by observation with an electron microscope.
    The method according to the invention is however just as applicable to natural materials whose particle size is greater than this range of values, and even when these particles have a diameter of one or more centimeters.
    In particular embodiments of the invention, the compression is carried out, at least during the heating step, at a pressure between 30 and 100 MPa, for example around 50 MPa.
    During the cooling step, compression of the material is preferably applied at the same pressure as during the heating step.
    Maintaining the compression of the material during the cooling step, and particularly in the range of values defined above, advantageously makes it possible to limit the porosity in the final material obtained, and consequently the quantity of water contained in this subject. This results in mechanical and structural solidity properties which are particularly good for the material obtained at the end of the implementation of the method according to the invention.
    In particular embodiments of the invention, the phase of heating the natural material to a temperature greater than or equal to the denaturation temperature of the scleroproteins is carried out for a sufficient time to ensure that all of the natural material subjected to heating has reached a temperature greater than or equal to the denaturation temperature of scleroproteins. A duration of the heating phase of between 1 and 45 minutes makes it possible to ensure it regardless of the dimensions of the part to be formed, and in particular its thickness.
    Depending on the thickness of the part, this duration of the heating phase can for example be between 1 and 20 minutes.
    The natural material in particulate form containing scleroproteins on which the process according to the invention is implemented preferably has a moisture content of between 0 and 20%, for example around 12%.
    Here the humidity level is defined, conventionally in itself, as the percentage by mass of water contained in the material, relative to the total mass of the material, under conditions of 60% relative humidity of air and at around 20 ° C. This humidity level can in particular be determined by comparing the weight of a sample of the material with the weight of this same sample after it has been subjected to a drying step at more than 100 ° C. until a weight is obtained. of the substantially constant sample.
    Where appropriate, the method according to the invention may include a prior step of drying the natural material, in order to obtain the desired humidity level.
    Prior to the implementation of the heating phase, the method according to the invention may include a step of mixing the natural material in particulate form with one or more additives, chosen according to the properties desired for the final part. Non-limiting examples of such additives are plasticizers, reinforcing fibers, dyes, etc.
    In particular embodiments of the invention, the natural material is not mixed with any other component for the implementation of the method according to the invention.
    In other particular embodiments of the invention, prior to the implementation of the heating phase, the method according to the invention comprises a step of mixing the natural material in particulate form with one or more additives, these additives being present in the mixture in an amount of less than 10% by weight, preferably less than 5% by weight, relative to the total weight of the mixture.
    Particularly preferred additives in the context of the invention are plasticizing agents, such as glycerol, and coloring substances, such as pigments, for example iron oxide.
    The natural material may for example be obtained from horn, hoof, hoof, wool, hair, feather or leather, animals.
    The scleroproteins contained therein are for example essentially keratin scleroproteins.
    The method according to the invention proves to be particularly advantageous for the manufacture of a part from a natural material in particulate form containing proteins derived from mammalian horn, for example from cow horn, or from leather of non-human animal.
    According to another aspect, the present invention relates to a part obtained by a manufacturing process according to the invention, meeting one or more of the characteristics described above.
    The material that makes up this piece has a lower hygroscopy, that is to say a lower tendency to absorb moisture from the air, than the original natural material. Thus, under identical relative humidity and temperature conditions, the moisture content of the final material obtained by the process according to the invention is lower than the moisture content of the initial natural material.
    In particular embodiments of the invention, the material which constitutes this part has a humidity level of between 0 and 20%, preferably less than 10%, and preferably less than 5%, under conditions of 60% relative humidity and at a temperature of 20 ° C.
    This part may in particular have been obtained by implementing the method according to the invention from natural material based on scleroproteins of any non-human animal origin.
    It may in particular have been obtained by implementing the method according to the invention on a material derived from mammalian horn, or alternatively on a material derived from non-human animal leather.
    Its density is greater than that of the original natural material. In the case where it was obtained from mammalian horn, and in particular from cow horn, it preferably has a density greater than or equal to 1.30 g / cm 3 .
    According to another aspect, the invention relates to the use of a part according to the invention, meeting one or more of the above characteristics, for the manufacture of an eyewear, jewelry or tableware, especially as a cutlery handle.
    More generally, the part according to the invention is particularly suitable for the manufacture of luxury objects and accessories, of watches, of jewelry, etc.
    It can also be used for the manufacture of marquetry articles, or for the ornament of shooting or hunting weapons, or for any other desired application.
    The characteristics and advantages of the invention will appear more clearly in the light of the examples of implementation below, provided for illustrative purposes only and in no way limit the invention, with the support of FIGS. 1 to 9, in which:
    - Figure 1 shows a graph representing the denaturation temperature of proteins contained in a cow horn sample as a function of its humidity, measured by differential scanning calorimetry;
    - Figure 2 shows a graph representing the results of dynamic mechanical analysis (Young's modulus and tan δ) as a function of temperature, of a material obtained by high pressure uniaxial molding of cow horn at 200 ° C and 100 MPa;
    - Figure 3 shows a graph representing, as a function of time, the temperature and the compression applied during the implementation of a flash sintering process according to the invention from cow's horn powder, the pressure being expressed in terms of displacement of the pistons of the flash sintering device;
    - Figure 4 shows a photograph of a pellet obtained by a flash sintering process according to the invention from cow's horn powder;
    - Figure 5 shows a graph representing the water adsorption isotherms for raw cow's horn (“Raw horn”), this cow's horn after grinding (“Powder”), and the material obtained from this powder by a high pressure thermomolding process according to the invention (“HPHT”);
    - Figure 6 shows the spectra obtained by FTIR infrared spectroscopy for raw cow's horn (“Raw horn”), this cow's horn after grinding (“Horn in powder”), the material obtained from this powder by a flash sintering process according to the invention ("SPS") and the material obtained from this powder by a high pressure thermomolding process according to the invention ("HPHT");
    - Figure 7 shows a graph representing, for raw cow's horn (“Raw horn”), this cow's horn after grinding (“Powder”), the material obtained from this powder by a conforming flash sintering process to the invention (“SPS”) and the material obtained from this powder by a high pressure thermomolding process according to the invention (“HPHT”), the variation of energy as a function of temperature, measured by differential scanning calorimetry;
    - Figure 8 shows an X-ray diffraction diagram obtained for raw cow's horn ("Horn"), the material obtained from this powder by a flash sintering process according to the invention ("SPS") and the material obtained from this powder by a high pressure thermomolding process according to the invention ("HPHT");
    - And Figure 9 shows photographs a / of a sample of non-human animal leather in particulate form, and b / of a part obtained from this sample by a flash sintering process according to the invention .
    A / Implementation of the process on cow horn
    The examples below are implemented from Aubrac cow horn.
    The natural horn is subjected beforehand to a grinding step, to form a horn powder whose particles have a diameter of between 200 and 500 μm.
    The density of the raw horn is 1.28 ± 0.01 g / cm 3 .
    The curve representing the denaturation temperature of the proteins contained in this cow horn powder, as a function of the humidity level of the powder, is established by differential scanning calorimetry (DSC) using a DSC1 instrument (Mettler-Toledo ), with medium pressure steel capsules of 80 pL, at 10 ° C / min.
    The result obtained is shown in Figure 1.
    It is observed, for example, that at a humidity rate of 9.6% (this rate can be obtained after drying the horn at 40 ° C), the protein denaturation temperature is around 185 ° C.
    Furthermore, the glass transition temperature of the denatured proteins is determined by dynamic mechanical analysis (DMA), using a Tritec 2000 DMA device (Triton Technology Ltd), simple embedding, 2 ° C / min.
    For this purpose, the horn powder at a humidity rate of 11.7% is subjected to high pressure uniaxial molding, at 200 ° C and 100 MPa for 3 min, using a MAPA 50 instrument (Pinette Emidecau Industries ), in a 5 cm square mold.
    The glass transition temperature of the material (reconstituted horn) thus obtained is measured by dynamic mechanical analysis.
    The result obtained is shown in Figure 2.
    It is noted that the glass transition temperature of the material, after denaturation of the proteins which constitute it, is 95 ° C.
    The material used for the experiments below has a humidity rate of 11.7% to 60% relative humidity of the air and a temperature of 20 ° C. At this humidity, the protein denaturation temperature is 181 ° C at atmospheric pressure
    EXAMPLE 1 Method by Flash Sintering
    A method according to the invention is used for the manufacture of a cylindrical part 160 mm in diameter and 22 mm in height, from horn powder.
    The tools used consist of a matrix and graphite pistons. The dimensions of the matrix are as follows:
    - outside diameter: 230 mm
    - inner diameter: 160 mm.
    The inner bore of the matrix is covered with a flexible graphite sheet, the function of which is to seal the assembly, and to prevent seizure between the matrix and the pistons. A graphite sheet is also positioned on the surfaces of the pistons in contact with the powder, to prevent the sintered material from sticking to the pistons.
    The desired quantity of powder is introduced into the matrix, which is then closed by the two pistons. The assembly is then placed in the enclosure of the flash sintering device (Sumitomo Sinter 2000), which is put under reduced pressure, at 5-10 Pa. The device is then programmed to apply compression to the matrix containing the powder. a pressure of 32 MPa in 4 min.
    Simultaneously, the assembly is heated by the Joule effect by an electric current passing through the pistons and passing through the walls of the graphite matrix. The whole is brought to 150 Ό in 7 min. The temperature control being carried out thanks to a thermocouple inserted on the external wall of the matrix. At this temperature, at this reduced pressure, the proteins used in the constitution of the powder undergo the phenomenon of denaturation.
    The temperature is maintained at 150 ° C for 10 min, after which the heating is switched off. Compression is maintained until the temperature inside the matrix reaches a value of 70 ° C, lower than the glass transition temperature of denatured proteins. The device is then opened, and the formed part is removed from the matrix.
    FIG. 3 shows the temperature and compression profiles of the matrix containing the material, which are applied as a function of time (the compression profile being expressed in terms of displacement of the pistons).
    It is observed that after 10 min of maintaining the temperature in the matrix at 150 ° C, the temperature gradually decreases. At the same time, the compression exerted on the matrix is substantially constant, the displacement of the pistons, by a few millimeters, being due to changes in the state of the material inside the matrix.
    At the end of the process, a densified horn pellet of the desired shape, of an intense black color, is obtained. This part is shown in figure 4.
    EXAMPLE 2 Method by High Pressure Thermomolding (HPHT)
    The device used is a MAPA 50 instrument (Pinette Emidecau Industries).
    The powder is placed in a rectangular mold of dimensions 5 x 1 cm, at a temperature of 200 ° C, higher than the denaturation temperature of proteins. It is then compressed, at this temperature, at a pressure of 100 MPa, for 5 min. The whole is then cooled to a temperature of 90 ° C., lower than the glass transition temperature of the denatured proteins, always under compression, before demolding.
    The material obtained at the end of the process is dark, and denser than the initial rough horn: the density of this material is 1.31 ± 0.02 g / cm 3 .
    Example 3 - Material characterizations
    Water adsorption isotherms
    The water adsorption isotherms are established by the dynamic vapor sorption technique (DVS), using a DVS Advantage (Surface Measurements Systems) instrument, at 5% to 95% relative humidity, with an interval of 10% and at 25 ° C, for: raw cow's horn (piece of horn of about 300 mg), the same horn after grinding (particle diameter between 200 and 500 pm), and the material obtained by a HPHT process according to the invention in Example 2 above.
    The results obtained are shown in Figure 5.
    There is very clearly an increase in the hygroscopy of the native horn after grinding. This is mainly related to the increase in the specific surface of the material.
    Then, after transformation by high pressure thermomolding in accordance with the present invention, the opposite effect is observed. The denaturation of scleroproteins has caused a marked reduction in hygroscopy (3% of water adsorbed at 60% relative humidity, against 7% for natural raw horn for example). This could be due to the deployment on the surface of more hydrophobic amino acids during the modification of the secondary structures of scleroproteins induced by the process according to the invention.
    Infrared soectroscopy
    An analysis by Fourier transform infrared spectroscopy (FTIR) is carried out, using a Spectrum 65 instrument (PerkinElmer), for: the raw cow's horn, the same horn after grinding, the material obtained by a flash sintering process (SPS) according to the invention in Example 1 above and the material obtained by an HPHT process according to the invention in Example 2 above.
    The results obtained are shown in Figure 6.
    We observe in this figure a modification of the frequency of vibration of the amide band I: 1633 cm −1 for the native horn and 1627 cm −1 for the horn after SPS treatment and 1628 cm −1 for the horn after HPHT treatment. This modification is characteristic of the modification of the secondary structure of keratin during the implementation of the method according to the invention.
    The amide II band (around 1530 cm ' 1 ) is, for its part, relatively relative to the environment of the NH groups, and the drop in intensity observed at 1540 cm' 1 could be relative to a decrease in the hydrogen bonds of these groups after transformation by the process according to the invention.
    PSC analyzes
    For each of the following materials: raw horn (in the form of a piece of approximately 20 mg), the same horn after grinding (particle diameter between 200 and 500 μm), the material obtained by an SPS process in accordance with invention in Example 1 above and the material obtained by an HPHT process according to the invention in Example 2 above, an analysis is carried out by differential scanning calorimetry (DSC) by means of a DSC1 instrument (Mettler-Toledo), with medium pressure steel capsules of 80 pL, at 10 ° C / min.
    We obtain for each material the curve representing the energy variation as a function of the temperature shown in Figure 7.
    These results confirm that the peaks materializing the endothermic phenomenon associated with the denaturation of proteins, present on the curves for the samples of untreated horn (these peaks being indicated by arrows in the figure) do not appear on the curves of the samples obtained after treatment of the horn by a method according to the invention. This confirms that the proteins contained in the materials obtained by methods in accordance with the invention have all been denatured during the implementation of these methods.
    X-ray diffraction analysis
    For each of the following materials: raw horn (in the form of a piece of approximately 20 mg), the material obtained by an SPS process in accordance with the invention in Example 1 above and the material obtained by an HPHT process in accordance with the invention in Example 2 above, an X-ray diffraction analysis (XRD) is carried out using a Bruker D8 Advance instrument.
    The curve shown for Figure 8 is obtained for each material.
    The absence of diffraction peaks on these diagrams, and the mere presence of a diffusion signal linked to the particular structure of the horn, demonstrate that the final material obtained by the process according to the invention is mainly amorphous.
    In addition, nitrogen absorption / desorption experiments show that the physical structure of the materials obtained both by the SPS process and by the HPHT process, implemented in accordance with the invention, approximates that of an elastic matrix. with different communicating porosity networks (micro / meso / macroscopic). The observation of these materials under the optical microscope and the scanning electron microscope confirms this hypothesis.
    B / Implementation of the process on leather
    This example is implemented using leather from scraping, in the form of crushed fiber whose particle size is between 100 and 250 μm.
    FIG. 9 shows, in a /, a photograph of the natural starting material.
    This material is subjected to a flash sintering process according to the invention. The operating protocol is similar to that described in Example 1 above, except that the heating temperature is 140 ° C. Under the conditions applied, the scleroproteins contained in the initial material are denatured.
    At the end of the process, the part shown in b / in FIG. 9 is obtained. This part has the appearance of natural leather, and improved properties compared to the natural starting material.
    权利要求:
    Claims (16)
    [1" id="c-fr-0001]
    1. A method of manufacturing a part, from a natural material in particulate form containing scleroproteins, characterized in that it comprises:
    a phase of heating said natural material under compression to a pressure greater than or equal to 30 MPa, to a temperature greater than or equal to the denaturation temperature of said scleroproteins,
    - And a cooling phase of the material thus obtained, called denatured material, to a temperature below 100 ° C, said compression being maintained for at least part of the cooling phase.
    [2" id="c-fr-0002]
    2. The method of claim 1, wherein the cooling phase of the denatured material is carried out to a temperature below the glass transition temperature of said denatured material.
    [3" id="c-fr-0003]
    3. Method according to any one of claims 1 to 2, according to which the heating phase of said natural material is carried out by flash sintering.
    [4" id="c-fr-0004]
    4. Method according to any one of claims 1 to 3, according to which the compression is carried out at a pressure between 30 and 100 MPa.
    [5" id="c-fr-0005]
    5. Method according to any one of claims 1 to 4, according to which the heating phase of said natural material to a temperature greater than or equal to the denaturation temperature of scleroproteins is carried out for a period of between 1 and 45 minutes.
    [6" id="c-fr-0006]
    6. Method according to any one of claims 1 to 5, wherein the particles of said natural material in particulate form have a diameter between 20 and 500 pm.
    [7" id="c-fr-0007]
    7. Method according to any one of claims 1 to 6, comprising a prior step of grinding said natural material.
    [8" id="c-fr-0008]
    8. A method according to any one of claims 1 to 7, wherein said natural material in particulate form containing scleroproteins has a humidity level between 0 and 20% under conditions of 60% relative humidity of the air and a temperature of 20 ° C.
    [9" id="c-fr-0009]
    9. Method according to any one of claims 1 to 8, according to which said scleroproteins are keratin proteins.
    [10" id="c-fr-0010]
    10. A method according to any one of claims 1 to 8, wherein said natural material in particulate form containing scleroproteins is of non-human animal origin.
    [11" id="c-fr-0011]
    11. Method according to any one of claims 1 to 10, according to which said natural material in particulate form containing scleroproteins is derived from mammalian horn.
    [12" id="c-fr-0012]
    12. Method according to any one of claims 1 to 10, according to which said natural material in particulate form containing scleroproteins is derived from non-human animal leather.
    [13" id="c-fr-0013]
    13. Part obtained by a manufacturing process according to any one of claims 1 to 12, characterized by a hygroscopy of the material which constitutes it weaker than said natural material.
    [14" id="c-fr-0014]
    14. Part according to claim 13, obtained from natural material derived from mammalian horn and having a density greater than or equal to 1.30 g / cm 3 .
    [15" id="c-fr-0015]
    15. Part according to claim 13, obtained from natural material derived from non-human animal leather.
    [16" id="c-fr-0016]
    16. Use of a part obtained by a method according to any one of claims 1 to 12 for the manufacture of an eyewear, jewelry or tableware, in particular as a cutlery handle.
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    WO2016135415A1|2016-09-01|Method for producing a reconstituted-wood type material
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    EP0859041A1|1998-08-19|Combustible product prepared from industrial and domestic waste and proecess for preparing the same
    FR2663019A1|1991-12-13|Process for the preparation of solid agglomerates from consistent inorganic sludges
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    FR2784995A1|2000-04-28|Fuel product production, especially fuel pellet or log, comprises compacting mixture of wood particles and animal blood plasma binder
    同族专利:
    公开号 | 公开日
    WO2019077112A1|2019-04-25|
    US20200316825A1|2020-10-08|
    FR3072680B1|2020-11-06|
    EP3697848A1|2020-08-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2001066159A1|2000-03-09|2001-09-13|Syntacoll Ag|Novel natural polymer-based material with improved properties for use in human and veterinary medicine and the method of manufacturing such|
    WO2007101171A2|2006-02-27|2007-09-07|Globus Medical, Inc.|Bone graft materials derived from mineralized gelatin|
    KR100825085B1|2007-04-02|2008-04-25|더페이스샵코리아|Cosmetic compositions comprising hydrolysis collagen peptide stabilized in nano-liposome and eucommia ulmoides oliver extract|
    KR100849020B1|2007-04-02|2008-07-29|더페이스샵코리아|Cosmetic compositions comprising hydrolysis collagen peptide stabilized in nano-liposome|
    KR20100042182A|2008-10-15|2010-04-23|더페이스샵코리아|A anti-aging cosmetic composition containing hydrolysis collagen peptide stabilized in nano-liposome and vitamin c|
    WO2012069736A1|2010-11-23|2012-05-31|Institut National Polytechnique De Toulouse |Process for manufacturing an eco-compatible solid material and eco-compatible solid material obtained|
    US20160375176A1|2014-01-28|2016-12-29|Beijing Allgens Medical Science And Technology Co., Ltd.|Mineralized collagen composite bone cementing and filling material|
    US20170112963A1|2015-10-26|2017-04-27|Theodore Malinin|Bone putty and gel systems and methods|
    FR3104058A1|2019-12-09|2021-06-11|Sintermat|Process for manufacturing a solid part by hot sintering treatment of at least one solid organic material|
    FR3106835A1|2020-02-03|2021-08-06|Authentic Material|PROCESS FOR THE PREPARATION OF A POWDER OF A MATERIAL OF NATURAL ORIGIN AND POWDER OBTAINED BY SUCH A PROCESS|
    FR3110485A1|2020-05-20|2021-11-26|Api'up|PROCESS FOR MANUFACTURING COMPOSITE PARTS FROM LEATHER, PRODUCTS OBTAINED|
    法律状态:
    2019-04-26| PLSC| Publication of the preliminary search report|Effective date: 20190426 |
    2019-10-29| PLFP| Fee payment|Year of fee payment: 3 |
    2020-11-02| PLFP| Fee payment|Year of fee payment: 4 |
    2020-12-11| CD| Change of name or company name|Owner name: TOULOUSE TECH TRANSFER, FR Effective date: 20201103 Owner name: INSTITUT NATIONAL POLYTECHNIQUE DE TOULOUSE, FR Effective date: 20201103 Owner name: CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE, FR Effective date: 20201103 Owner name: AUTHENTIC MATERIAL, FR Effective date: 20201103 Owner name: INSTITUT NATIONAL DE RECHERCHE POUR L'AGRICULT, FR Effective date: 20201103 |
    2021-10-28| PLFP| Fee payment|Year of fee payment: 5 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1759886|2017-10-20|
    FR1759886A|FR3072680B1|2017-10-20|2017-10-20|PROCESS FOR MANUFACTURING A PART FROM A PARTICULAR NATURAL MATERIAL AND PART OBTAINED BY SUCH A PROCESS|FR1759886A| FR3072680B1|2017-10-20|2017-10-20|PROCESS FOR MANUFACTURING A PART FROM A PARTICULAR NATURAL MATERIAL AND PART OBTAINED BY SUCH A PROCESS|
    PCT/EP2018/078717| WO2019077112A1|2017-10-20|2018-10-19|Method for producing a part from a particulate natural material and part obtained by such a method|
    EP18793628.1A| EP3697848A1|2017-10-20|2018-10-19|Method for producing a part from a particulate natural material and part obtained by such a method|
    US16/652,591| US20200316825A1|2017-10-20|2018-10-19|Method for producing a part from a particulate natural material and part obtained by such a method|
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