WO2010058049A1 - Préparation de matériaux biocompatibles à partir de déchets issus du processus de fabrication de la bière, et utilisations de ces matériaux - Google Patents

Préparation de matériaux biocompatibles à partir de déchets issus du processus de fabrication de la bière, et utilisations de ces matériaux Download PDF

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Publication number
WO2010058049A1
WO2010058049A1 PCT/ES2009/070475 ES2009070475W WO2010058049A1 WO 2010058049 A1 WO2010058049 A1 WO 2010058049A1 ES 2009070475 W ES2009070475 W ES 2009070475W WO 2010058049 A1 WO2010058049 A1 WO 2010058049A1
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Prior art keywords
final temperature
material obtained
temperature
stage
beer
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PCT/ES2009/070475
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English (en)
Spanish (es)
Inventor
Malcolm Yates Buxcey
Maria De Los Angeles Martin Luengo
María Blanca CASAL PIGA
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Consejo Superior De Investigaciones Cientificas (Csic)
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Publication of WO2010058049A1 publication Critical patent/WO2010058049A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/12—Phosphorus-containing materials, e.g. apatite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
    • B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
    • B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
    • B01J27/1806—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with alkaline or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/084—Decomposition of carbon-containing compounds into carbon
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

Definitions

  • the present invention relates to a method of obtaining biocompatible material from the drying and heat treatment of beer bagasse, as well as its use in bone tissue engineering. Therefore, from the point of view of the process, the present invention falls within the sector of the synthesis and preparation of new materials. Regarding its applications or uses, the invention falls within the health sector, and more specifically in bone tissue implants.
  • the average age of the population The current development of tissue engineering is based both on the development of cultures of more or less pluripotential cell lines, inducing and regulating factors of cell differentiation, and on the development of matrices with support and structure capacity. Specifically in the development of bone regeneration, multiple models of osteoconductive characteristics, rich in phosphocalcic contents, have been designed.
  • Biomaterials used must have the appropriate characteristics of composition, mechanical strength, porosity, degradation rate in the appropriate biological solutions, material transport properties and exchange of nutrients and waste products, using polymers, proteins and inorganic materials (alumina, zirconia, hydroxyapatite, calcium phosphates and bioactive glasses), mainly.
  • polymers, proteins and inorganic materials alumina, zirconia, hydroxyapatite, calcium phosphates and bioactive glasses
  • the solids used are synthetic (AL Oliveira, PB Malafaya, RL Reis (2003), Sodium silicate gel as a precursor for the in vitro nucleation and growth of a bone-like apatite coating in compact and porous polymeric structures, Biomaterials, 24, 2575-2584), (AG Dias, IR Gibson, JD Santos, MA Lopes (2007), Physicochemical degradation studies of calcium phosphate glass ceramic in the CaO-P2O5-MgO-TiO2 system, Acta Biomaterialia, 3, 263-269) or of animal origin, although recently the diseases related to the bovine population have raised the fear among human beings in implanting materials with such origin, being more recommended the use of materials of non-animal origin.
  • Synthetic materials are often obtained by complicated synthesis of a large number of synthetic steps, using toxic reagents (eg benzoyl peroxide, benzene, anilines), with calcinations at very high temperatures close to 1500 0 C , to produce bioceramic materials, to which silicon is added to finish, by hydrolysis of TEOS, with a final sintering step at more than 1100 0 C.
  • toxic reagents eg benzoyl peroxide, benzene, anilines
  • the present work is based on obtaining biocompatible solids of added value using as raw material by-products of agricultural origin, carrying out processes consistent with sustainable development, that is, avoiding the use of toxic substances or procedures.
  • the structure of the Final materials can be designed by changing the variables of the preparation process, so that they can be used in cell growth, according to their final textural and crystalline characteristics.
  • the present invention is based on three fundamental aspects: 1) the obtaining of materials comprising phosphates and silicates, by drying and heat treating the bagasse (previous residues of the beer manufacturing process), 2) the material obtained by this procedure 3) its use in bone tissue engineering, as well as its use as a catalyst.
  • the present invention is based on a process, developed by the inventors, to obtain biocompatible materials comprising phosphates and silicates from bagasse residues of beer.
  • the materials obtained given their similarity to the bone mineral phase, are suitable for bone tissue engineering.
  • one aspect of the present invention is the process of obtaining materials comprising phosphates and silicates, hereinafter the method of the invention, by drying and heat treating the bagasse of beer.
  • beer bagasse is defined as the byproduct of
  • the beer industry resulting from the pressing and filtering of the must obtained from the malted barley grain, after its saccharification.
  • the bagasse of beer has a large amount of liquid, due to the processing of the original materials, and a dry matter content of 20-25%.
  • a preferred aspect of the present invention is the process of the invention that is developed through the steps of: i) Drying of beer bagasse by heating from room temperature to 100-200 0 C with a temperature ramp between 1 and 10 ° C / min and maintaining the final temperature for at least two hours to stop the fermentation of the original solid. ii) Treatment of the resulting solid in i) from room temperature to a temperature within the range of 350-1200 0 C, maintaining the final temperature for more than 1 hour
  • a more preferred aspect of the present invention is the process of the invention in which the final temperature of stage i) is 15O 0 C.
  • Another more preferred aspect of the present invention is the process of the invention in which the final temperature of stage ii) is 85O 0 C, giving rise to a material comprising phosphorus, silicon, calcium and magnesium as main elements, in addition to lower amounts of sodium and potassium.
  • the material obtained by the process of the invention, using this final temperature of 85O 0 C can be used in bone tissue engineering.
  • Another more preferred aspect of the present invention is the process of the invention in which the heating ramp used in i) is 5 ° C / min.
  • Another more preferred aspect of the present invention is the process of the invention in which the final temperature in stage i) is maintained for 4 hours.
  • Another more preferred aspect of the present invention is the process of the invention in which the final temperature in stage ii) is maintained for 2 hours.
  • Another more preferred aspect of the present invention is the process of the invention in which the final temperature of stage ii) is 35O 0 C, giving rise to a material comprising carbon, phosphorus, silicon, calcium and magnesium, in addition to amounts lower sodium and potassium.
  • the material obtained by the process of the invention, using this final temperature of 35O 0 C can be used as a catalyst, absorber or semiconductor.
  • Another aspect of the present invention is the material obtained by the process of the invention, hereinafter material of the invention.
  • material of the invention The observation of the material of the invention with X-ray diffraction determines a crystalline structure corresponding to calcium and magnesium phosphates and silicates. Textural analysis of the material of the invention indicates the presence of macropores above 100 microns and a specific area of around 8m 2 / g. The results of chemical analysis and microwave analysis confirm the presence of phosphorus, silicon, calcium and magnesium as the main elements of the material of the invention, in addition to lower amounts of sodium and potassium.
  • Another preferred aspect of the invention is the material of the invention characterized in that it mostly comprises phosphorus, silicon, calcium and magnesium, in addition to lower amounts of sodium and potassium.
  • the material of the invention is suitable for the engineering of bone tissues and also its content in ions present in the physiological environment (sodium, calcium, magnesium, potassium) makes it highly biocompatible.
  • ions present in the physiological environment sodium, calcium, magnesium, potassium
  • the presence of phosphorus, silicon and magnesium is beneficial for tissue engineering, since phosphates are usually more soluble in biological fluids than hydroxyapatite.
  • the presence of silicon is used to modify the dissolution capacity of the biomaterial, having found a greater dissolution of silicon ions and faster reabsorption in silica-calcium phosphate composites than in materials without silica.
  • biologically active cations such as magnesium is a contributing factor in the properties of this type of biomaterials, since it influences the process of the subsequent biomineralization of the solid.
  • Bioreabsorbable materials are important for tissue regeneration, since they do not require a second operation to remove the implant.
  • Another aspect of the present invention is the use of the material of the invention in bone tissue engineering
  • the material of the invention given its biocompatibility and its textural characteristics with pore diameters of several hundred microns, which can be modified by procedures designed in this regard, is useful for the growth of fat stem cells.
  • a renewable material given its origin of agricultural waste, after the necessary modifications, is used for the cultivation of stem cells from fat.
  • Natural coral-based materials have been used for similar purposes, although their sustainability is doubtful, since coral materials cannot be considered renewable and their presence is very important for the balance of the environment where they develop.
  • the plant origin of the material of the invention from residues of the agricultural industry, prevents the possible spread of diseases that can be transmitted through the bone mass of animals.
  • the material of the invention contains silicon in its composition, so it is not necessary to add it to modify the hardness and biodegradability of the final biomaterials, with the consequent economic benefit.
  • Another aspect of the present invention is the use of the material of the invention as a catalyst.
  • EXAMPLE 1 Preparation of biocompatible material from beer bagasse and characterization to verify its application in bone tissue engineering.
  • the material obtained mainly comprises phosphorus, silicon, calcium and magnesium as the main elements, as well as lower amounts of sodium and potassium.
  • the influence of its structural, surface, textural and biocompatibility characteristics on the growth of fat stem cells has been studied.
  • X-ray powder diffraction was used with an X ' Pert Pro PANalytical Polycrystalline diffractometer.
  • X-ray diffraction diagrams were made, with peaks between 22 and 25 ° and at 31, 33 and 34.5 2 ⁇ corresponding to tricalcium phosphate (PDF 09-0348) and calcium silicate at 29.5 ° 2 ⁇ (PDF 01 -1029).
  • the apparent specific surfaces were obtained according to the BET method, assuming an area for the nitrogen molecule of 0.162 nm 2 .
  • Particle size and meso and macropore distributions were determined by mercury intrusion porosimetry, after drying the samples in an oven at 150 ° C for 16 hours. For these measurements, a mercury contact angle of 141 ° and a surface tension of 484 mNm "1 according to IUPAC recommendations are assumed as standard.
  • the adsorption of nitrogen in the samples gives rise to type II isotherms.
  • the curve obtained in the measure of mercury intrusion porosimetry indicates particle sizes of several hundred microns.
  • the porosity study reveals that the material has an open pore structure, with more than 80% of them between 100 and 300 microns in diameter.
  • the bulk density of the material is 0.35 g / cc, indicating that it has a porosity of 86%.
  • the skeletal density is 2.5 g / cc.
  • the porosity of similar solids, taken for comparison in bibliographic searches is usually in a range of 50 to 500 microns.
  • the results of textural characterization confirm that depending on the parameters used for the design of the solids, they have the capacity to serve as scaffolds in cell growth, which are confirmed by analysis performed with scanning electron microscopy.
  • FTIR infrared spectroscopy
  • FTIR infrared spectroscopy
  • EXAMPLE 2 Preparation of biocompatible material from beer bagasse and characterization to verify its application as a catalyst, substance absorber or semiconductor.
  • the beer bagasse obtained directly from the MAHOU factory in Alovera, Guadalajara, is dried by heating from room temperature to 15O 0 C with a temperature ramp of 5 ° C / min and maintaining the final temperature for four hours to stop the Ia fermentation of the original solid. Then, the resulting solid was heated from room temperature to a temperature of 350 0 C, maintaining the final temperature for 2 hours.
  • the texture of this material was determined by the nitrogen adsorption-desorption technique in a Micromeritics ASAP 2010 equipment with N 2 at 77 K, subjecting the solid previously to an evacuation process for 16 hours at 300 0 C to eliminate any species that It could be weakly adsorbed on the surface.
  • the apparent specific surfaces (S BET ) were obtained according to the BET method, assuming an area for the nitrogen molecule of 0.162 nm 2 [Rouquerol, F., Rouquerol J., Sing, K .; Adsorption by powders and porous solids- principies, methodology and applications, (1999), Academic Press, London].
  • X-ray powder diffraction was used with an X ' Pert Pro PANalytical Polycrystalline diffractometer.
  • the material obtained mainly comprises carbon, phosphorus, silicon, calcium and magnesium as the main elements, as well as lower amounts of sodium and potassium.
  • S BET specific surface area

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Epidemiology (AREA)
  • Thermal Sciences (AREA)
  • Dermatology (AREA)
  • Physics & Mathematics (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Materials For Medical Uses (AREA)

Abstract

La présente invention concerne un procédé d'obtention de matériaux biocompatibles comprenant des phosphates et des silicates, à partir de déchets issus de l'industrie agroalimentaire, et notamment à partir du séchage et du traitement thermique de la drêche de brasserie, résidu provenant de la fabrication de la bière. L'invention concerne également l'utilisation de ces matériaux biocompatibles en ingénierie des tissus osseux.
PCT/ES2009/070475 2008-11-21 2009-10-29 Préparation de matériaux biocompatibles à partir de déchets issus du processus de fabrication de la bière, et utilisations de ces matériaux WO2010058049A1 (fr)

Applications Claiming Priority (2)

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ES200803331 2008-11-21
ESP200803331 2008-11-21

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WO2010058049A1 true WO2010058049A1 (fr) 2010-05-27

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1426066A1 (fr) * 2001-06-05 2004-06-09 Yenssen Biotech Co., Ltd. Produit d'echafaudage dans le domaine du genie tissulaire osseux humain, ses procedes de preparation et ses applications
EP1584338A2 (fr) * 2004-04-07 2005-10-12 Millenium Biologix Inc. Compositions d'oxyapatite substitées par le silicium

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1426066A1 (fr) * 2001-06-05 2004-06-09 Yenssen Biotech Co., Ltd. Produit d'echafaudage dans le domaine du genie tissulaire osseux humain, ses procedes de preparation et ses applications
EP1584338A2 (fr) * 2004-04-07 2005-10-12 Millenium Biologix Inc. Compositions d'oxyapatite substitées par le silicium

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CLARK ET AL.: "Catalytic performance of carbonaceus materials in the esterification of succinic acid catalysis.", COMMUNICATIONS, vol. 9, 2008, pages 1709 - 1714 *
DOSORETZ, C.G. ET AL.: "Removal of trace organics from water using pumped bed-membrane bioreactor with powdered activated carbon.", JOURNAL OF MEMBRANE SCIENCE, vol. 239, August 2004 (2004-08-01), pages 81 - 90 *
MAITI, S. ET AL.: "Silicon-doped carbon semiconductors fron rice husk char.", MATERIALS CHEMISTRY AND PHYSICS, vol. 109, 15 May 2008 (2008-05-15), pages 169 - 173 *

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