WO2009069164A1 - Matériaux nanocomposites hybrides pour le stockage d'hydrogène - Google Patents

Matériaux nanocomposites hybrides pour le stockage d'hydrogène Download PDF

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WO2009069164A1
WO2009069164A1 PCT/IT2008/000677 IT2008000677W WO2009069164A1 WO 2009069164 A1 WO2009069164 A1 WO 2009069164A1 IT 2008000677 W IT2008000677 W IT 2008000677W WO 2009069164 A1 WO2009069164 A1 WO 2009069164A1
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treating
solutions
nanocomposite material
preparation
carbon
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Inventor
Maria Letizia Terranova
Massimiliano Lucci
Silvia Orlanducci
Francesco Toschi
Emanuela Tamburri
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/0005—Reversible storage of hydrogen, e.g. by hydrogen getters or electrodes
    • C01B3/001—Reversible storage of hydrogen, e.g. by hydrogen getters or electrodes characterised by the uptaking media; Treatment thereof
    • C01B3/0018—Inorganic elements or compounds, e.g. oxides, nitrides, borohydrides or zeolites; Solutions thereof
    • C01B3/0021—Elemental carbon, e.g. active carbon, carbon nanotubes or fullerenes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/0005—Reversible storage of hydrogen, e.g. by hydrogen getters or electrodes
    • C01B3/001—Reversible storage of hydrogen, e.g. by hydrogen getters or electrodes characterised by the uptaking media; Treatment thereof
    • C01B3/0078—Composite solid storage media, e.g. mixtures of polymers and metal hydrides, coated solid compounds or structurally heterogeneous solid compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
    • H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
    • H01M8/04201—Reactant storage and supply, e.g. means for feeding, pipes
    • H01M8/04216—Reactant storage and supply, e.g. means for feeding, pipes characterised by the choice for a specific material, e.g. carbon, hydride, absorbent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2365/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/02—Polyamines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention concerns a new kind of materials for hydrogen storage and a process for their preparation.
  • the invention concerns hybrid nanocomposite materials for hydrogen storage, made of carbon nanostructures in a matrix made of a conductive polymer.
  • thermodynamics The main features required to the materials proposed for storing hydrogen are: - suitable adsorption and desorbing thermodynamics,
  • Main materials studied for hydrogen storage belong to five main classes: - metallic hydrides (A. Zuttel, Materials for hydrogen storage,
  • MOFs metal-organic frameworks
  • the class of metallic hydrides comprises a very high number of materials.
  • hydrides of intermetallic compounds give the best performances in terms of adsorbed hydrogen volumetric amount, while the percentage by weight ranges from 2 up to 10%. Nevertheless, desorption temperatures can be very high. Further, these materials are very heavy and can be easily polluted, and further they have high costs of production.
  • zeolites it is possible to operate at temperature and pressure conditions that are not too severe (temperatures of 20-200 0 C and pressures of 2-10MPa), but adsorbed hydrogen does not exceed 1.8%.
  • MOFs proposed as materials for hydrogen storage can adsorb hydrogen in an amount that is not higher than 4%, but only at very low temperature (77K).
  • PIMs polymer of intrinsic microporosity
  • the composition of these polymers can, in principal, be chemically varied and moduled. It is believed that adsorbing properties of these polymers exclusively depend on their microporosity. At present, using these polymers it is possible to reach an amount of adsorbed hydrogen of 2% by weight at 77K.
  • conductive polymers of the type of PANI (polyaniline) and PPY (polypirrole) proved to have a reversible adsorption ability of respectively 6% and 8% at environment temperature and pressure of 9,3MPa. Unfortunately, these results were not subsequently confirmed.
  • porous carbon materials raised a very high interest, thanks to the discover of nanostructured and/or nanometric carbon material such as nanotubes (CNT), nanofibres, fullerenes and nanoparticles.
  • nanostructured and/or nanometric carbon material such as nanotubes (CNT), nanofibres, fullerenes and nanoparticles.
  • nanocomposite materials In the formation of nanocomposite materials, the two components, generally known as matrix and filler, institute such relationships giving surprising features to the obtained material. For this reason the study and preparation of nanocomposite materials raised great scientific and technologic interest.
  • nanocomposites based on polymers and carbon nanotubes were successfully tested and used in mechanical, thermal and electronic applications. Storically, polymers always proved to act as inibitors with respect to gas adsorption because of the impossibility to reach micropores and/or their lack.
  • Conductive polymers and PIMs until now are the only materials that proved their ability in adsorbing hydrogen. Coupling these polymers with carbon nanometric materials, well known as gas adsorbing materials, can lead to the formation of extremely interesting nanocomposites.
  • Said materials are able to interact with gas, holding it in their interior and working in a range of temperature also comprising environment temperature, with storing time extremely fast in a range of pressure values also comprising environment pressure. Said materials are also capable of quickly releasing storaged hydrogen. Debonding times are in the range of one minute at environment temperature and even shorter if the system is heated, however always at a temperature lower than 100 0 C.
  • the aim of the present invention is therefore that of providing a new class of materials allowing to overcome the limits of the materials according to the prior art and to obtain the technical results previously described.
  • a further aim of the invention is that said materials can be realised with substantially limited costs.
  • a nanocomposite material for hydrogen storage made of a filler made of carbon nanostructures in a conductive polymeric matrix chosen amongst polyethylendioxytiophene (PEDOT), polypirrole (PPY), polyorthoanisydine (POA), polydiaminenaphthalenes (PDAN), polydiaminebenzenes (PDAB).
  • PEDOT polyethylendioxytiophene
  • PY polypirrole
  • POA polyorthoanisydine
  • PDAN polydiaminenaphthalenes
  • PDAB polydiaminebenzenes
  • said carbon nanostructures are chosen amongst: single wall carbon nanotubes (SWCNT), double wall carbon nanotubes (DWCNT), multiwall carbon nanotubes (MWCNT), nanowires and carbon nanofibres having a diametre shorter than 200 nm (NFC), carbon nanoparticles (amorphous or graphitic) having a diametre comprised between 10 and 500 nm (NPC), fullerenes (C 6 o).
  • SWCNT single wall carbon nanotubes
  • DWCNT double wall carbon nanotubes
  • MWCNT multiwall carbon nanotubes
  • NFC carbon nanoparticles (amorphous or graphitic) having a diametre comprised between 10 and 500 nm (NPC), fullerenes (C 6 o).
  • said carbon nanostructures are present in a concentration by weight comprised between 1% and 20% of the weight of the material.
  • said process further comprise a step, following the step of mixing between the polymer in solution and the nanometric material, of homogenising the polymer/nanomaterial dispersion in an ultrasound bath.
  • said process can further comprise a preliminar step of treatment of the carbon materials, chosen amongst:
  • said process for the preparation of a nanocomposite material provides for the use of electrochemical techniques with controlled potential, for the growing of each polymer. Further, according to the invention, said process provides for the use of solutions of monomers in concentration comprised between: 1mM and 10OmM and concentrations of carbon nanomaterial comprised between: 20 mg/l and 200 mg/l.
  • said process can further comprise a preliminar step of treatment of the carbon materials, chosen amongst:
  • said alternative process for the preparation of a nanocomposite material provides for the use of electrochemical techniques with controlled potential, for the growing of each polymer.
  • said further process provides for the use of solutions of monomers in concentration comprised between:
  • said process can further comprise a preliminar step of treatment of the carbon materials, chosen amongst:
  • Hybrid nanocomposite materials forming the object of the present invention have, with respect to the process of hydrogen storage/debonding, important advantages with regard to the single components constituting them. Further, such nanocomposites present a series of complimentary advantages typical of composite materials: - increased mechanical properties of the composite with respect to those of the polymer,
  • FIG. 1 shows a schematic view of the apparatus used for H 2 adsorption measures in the experimental tests made on some materials according to the present invention
  • - figures 2A and 2B show the quartzes of a microbalance respectively before and after the deposition of an adsorbing material according to the present invention
  • - figure 3 shows a photographic picture obtained with an optical microscope (con obiettivo 5Ox) of the film of polyethylendioxytiophene:polystirenesulphonate (PEDOTPSS) nanocomposite material with single wall carbon nanotubes (SWCNT), obtained according to the present invention
  • - figure 4 shows a photographic picture obtained with a scan electron microscope (SEM) of a polyethylendioxytiophene/single wall carbon nanotubes (PEDOT/SWCNT) nanocomposite material, obtained according to the present invention, wherein it is possible to see nanotubes in the polymeric matrix
  • - figure 5 shows a picture obtained with a STM microscope of a film of nanocomposite material based on polyorthoanisydine (POA) and multiwall carbon nanotubes (
  • - figure 6 shows examples of adsorption and desorption curves obtained at environment temperature and atmospheric pressure for films of nanocomposite material based on polyethylendioxytiophene:polystirenesulphonate and single wall carbon nanotubes treated in HNO 3
  • - figure 7 shows on a diagram the linear trend of the adsorption of the composite system polyorthoanisydine (POA) together with multiwall carbon nanotubes (MWCNT).
  • POA polyorthoanisydine
  • MWCNT multiwall carbon nanotubes
  • Hybrid nanocomposite material is made of an organic polymeric component belonging to the class of conductive polymers that can be chosen amongst the following: polyethylendioxytiophene (PEDOT), polypirrole (PPY), polyorthoanisydine (POA), polydiaminenaphthalenes (PDAN), polydiaminebenzenes (PDAB).
  • PEDOT polyethylendioxytiophene
  • PY polypirrole
  • POA polyorthoanisydine
  • PDAN polydiaminenaphthalenes
  • PDAB polydiaminebenzenes
  • the inorganic filler is a carbon nanometric material and can be chosen amongst the following: single wall carbon nanotubes (SWCNT), double wall carbon nanotubes (DWCNT), multiwall carbon nanotubes (MWCNT), nanowires and carbon nanofibres having a diametre shorter than 200 nm (NFC), carbon nanoparticles (amorphous or graphitic) having a diametre comprised between 10 and 500 nm (NPC), fullerenes (C 60 ).
  • SWCNT single wall carbon nanotubes
  • DWCNT double wall carbon nanotubes
  • MWCNT multiwall carbon nanotubes
  • NFC carbon nanofibres having a diametre shorter than 200 nm
  • NFC carbon nanoparticles (amorphous or graphitic) having a diametre comprised between 10 and 500 nm (NPC), fullerenes (C 60 ).
  • SWCNT SWCNT, DWCNT, MWCNT, NFC, NPC and C ⁇ o
  • SWCNT SWCNT, DWCNT, MWCNT, NFC, NPC and C ⁇ o
  • This method involves preparing a solution of polymer in a suitable solvent and its blending with a known amount of carbon nanomaterial.
  • the method provides for the use of an ultrasound bath, for homogenizing the polymer/nanomaterial dispersion.
  • the resulting nanocomposite can have concentrations by weight of carbon nanomaterial comprised between 1% and 20%.
  • the preparation of the nanocomposite material can be performed through electrochemical synthesis of the polymer with simultaneous inglobation of the nanometric material.
  • This method provides for the electrochemical deposititon of the polymer, starting from a solution of monomer in which carbon materials were dispersed.
  • electrochemical deposititon of the polymer starting from the monomer can be performed on a layer of nanocarbon materials previously deposited on the operating electrode.
  • the method provides for the electrochemical deposititon through the application of a suitable potential to the operating electrode.
  • the method provides for the use of electrochemical techniques with controlled potential. Potential is controlled to suitable values for the growing of each polymer.
  • Nanocomposite materials prepared according to one of the two different method previously shown, were subjected to the following determination hydrogen adsorption without further treatments and symulations. Hydrogen adsorption ,easure system
  • the method of preparation of the nanocomposite material through blending of the polymer in solution and the nanometric material provides for the deposition occurring directly on the device used for the determination of hydrogen adsorption.
  • Figure 1 shows a schematic view of the measuration device, in which the numeral 10 is used for an inert material room inside which a microbalance is positioned, and is respectfully linked to a H 2 c ylinder pointed as 11 and an inert gas cylinder 12, respectively through connecting lines on which fluximetres 13 are present. Fluximeters are controlled by a flux controller 14, operated by an electronic elaborator 15, to which data detected by the microbalance are conveyed after passage in a counter 16.
  • the measuration device used and shown in figure 1 worked at environment temperature. However, it is also possible to heat the system, in order to speed up the desorption step.
  • Adsorption/desorption measures shown in the following examples were performed in sequence, by measuring at first quartz alone, subsequently quartz on which adsorbing material was deposited and finally quartz with the adsorbing material after esposition to hydrogen. For the verification and quantification of hydrogen desorption it was proved that the mass of the sample decreased from time to time when subjected to a flux of an inert gas such as nitrogen, that is not adsorbed by the material in object.
  • an inert gas such as nitrogen
  • a solution was prepared comprised of 100ml of a polymer polyethylendioxytiophene:polystirenesulphonate (PEDOT.PSS) and a filler made of single wall carbon nanotubes (SWCNT), prelimina y treated with an acid solution of HNO 3 (150mg). An amount of 10 ⁇ l of this solution was deposited on the quartz surface used as microbalance (as shown in figures 2A and 2B). The system was maintained at 100 0 C for about 30 minutes.
  • Figure 3 shows a photografic pictuteres obtained with an optical microscope (5Ox magnifier) of the films of nanocomposite material prepared.
  • the sample was introduced in a measuration room made of inert material and was subjected for two hours to a nitrogen flux, to remove traces of other possible pollutants.
  • FIG. 6 shows on a diagram the adsorption and desorption curves obtained at environment temperature and atmospheric pressure. Diagram of figure 6 shows how the process is repeatible and completely reversible.
  • the amount of adsorbed hydrogen was of 4% by weight, with respect to the amount of filler (SWCNT) that is present in the nanocomposite material.
  • SWCNT filler
  • a solution was prepared comprised of a polymer PEDOTPSS
  • NPC (100ml) and 100mg of filler NPC.
  • the sample was introduced in the measurements rooms, inside which a flux of nitrogen was initially introduced, so to remove any traces of other possible pollutants. Subsequently, the sample was subjected to alternate flux hydrogen and nitrogen, so to verify the reversibility of the adsorption and desorption by means of an increase/decrease by weight.
  • the amount of adsorbed hydrogen measured with this system was of 3% by weight, with regard to the amount of filler intorduced in the nanocomposite.
  • a nanocomposite material made of PEDOT and SWCNT was prepared.
  • the sample was prepared through a synthesis/n situ, consisting in polymerisation starting from the respective monomer soluted in a solution wherein components of filler (SWCNT) to be included in the polymeric matrix were previously dispersed. Since this process of preparation is simply an electropolymerisation in acqueous mean, a preliminary treatment of SWCNT is necessary, so to introduce hydrophilic functions allowing the dispersion in the reaction means.
  • Figure 4 shows a photographic picture obtained with a scan electron microscope (SEM) of the nanocomposite material PEDOT/SWCNT. In the figure it is possible to see how the nanotubes link together different areas of the polymeric matrix.
  • SEM scan electron microscope
  • the electropolymerised sample was introduced in the measuration room and subjected for two hours at a flux of nitrogen, so to remove any traces of other possible pollutants.
  • the quartz covered by nanocomposite material was subjected to alternate fluxes of hydrogen and nitrogen, so to verify the reversibility of adsorption and desorption by means of an increase/decrease by weight.
  • the amount of adsorbed hydrogen of this system was comprised between 2 and 4% by weight with respect to the amount of filler introduced in the nanocomposite material.
  • a solution was prepared comprised of 100 ml of POA and 150 mg of filler of MWCNT.
  • Figure 5 shows a photographic picture obtained with a STM microscope of the films of nanocomposite material based on polyorthoanisydine (POA) and carbon nanotubes obtained. After drying, the sample was introduced in the measurement rooms made of inert material and was subjected for two hours at a flux of nitrogen, so to remove any traces of other possible pollutants.
  • POA polyorthoanisydine
  • the quartz covered by the nanocomposite material was subjected to alternate flux of hydrogen and nitrogen, so to verify the reversibility of the adsorption and desorption by means of an increase/decrease by weight.
  • Figure 7 shows the linear trend of the adsorption.
  • the amount of adsorbed hydrogen was 2-3% by weight with reference to the amount of filler (MWCNT) present in the nanocomposite material.
  • MWCNT filler

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Abstract

L'invention porte sur un matériau nanocomposite pour le stockage d'hydrogène, composé d'une charge constituée de nanostructures de carbone dans une matrice polymère conductrice choisie parmi le polyéthylènedioxythiophène (PEDOT), le polypyrrole (PPY), la polyorthoanisidine (POA), les polydiaminenaphtalènes (PDAN), les polydiaminebenzènes (PDAB). L'invention porte en outre sur des procédés pour la préparation dudit matériau.
PCT/IT2008/000677 2007-11-28 2008-10-30 Matériaux nanocomposites hybrides pour le stockage d'hydrogène Ceased WO2009069164A1 (fr)

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EP08854854A EP2223369A1 (fr) 2007-11-28 2008-10-30 Matériaux nanocomposites hybrides pour le stockage d'hydrogène

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ITRM2007A000618 2007-11-28
IT000618A ITRM20070618A1 (it) 2007-11-28 2007-11-28 Materiali nanocompositi ibridi per lo stoccaggio di idrogeno.

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Cited By (4)

* Cited by examiner, † Cited by third party
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EP1720931A4 (fr) * 2004-02-26 2007-08-08 Fpinnovations Polymeres a base d'epichlorohydrine contenant des groupes amino primaires utilises comme additifs dans la fabrication du papier
US9085463B2 (en) 2011-01-17 2015-07-21 Marelle, Llc Water-soluble functionalized fullerenes
ES2570391A1 (es) * 2016-01-18 2016-05-18 Univ Cartagena Politecnica ABS dopado con grafeno
IT201600128191A1 (it) * 2016-12-19 2018-06-19 Nanoshare Soc A Responsabilita Limitata Uso di nanocarbonio derivato da shungite in materiale polimerico per lo stoccaggio di idrogeno

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