US20060292054A1 - Mesostructured aluminosilicate material - Google Patents

Mesostructured aluminosilicate material Download PDF

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US20060292054A1
US20060292054A1 US11/159,384 US15938405A US2006292054A1 US 20060292054 A1 US20060292054 A1 US 20060292054A1 US 15938405 A US15938405 A US 15938405A US 2006292054 A1 US2006292054 A1 US 2006292054A1
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mesostructured
surfactant
material according
precursor
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Alexandra Chaumonnot
Aurelie Coupe
Clement Sanchez
Patrick Euzen
Cedric Boissiere
David Grosso
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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Priority to US11/204,774 priority Critical patent/US20060143144A1/en
Priority to US11/203,900 priority patent/US20060179116A1/en
Priority to US11/206,308 priority patent/US20060149408A1/en
Priority to US11/207,618 priority patent/US20060161895A1/en
Assigned to INSTITUT FRANCAIS DU PETROLE reassignment INSTITUT FRANCAIS DU PETROLE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BOISSIERE, CEDRIC, CHAUMONNOT, ALEXANDRA, COUPE, AURELIE, EUZEN, PATRICK, GROSSO, DAVID, SANCHEZ, CLEMENT
Publication of US20060292054A1 publication Critical patent/US20060292054A1/en
Priority to US12/408,437 priority patent/US7851320B2/en
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    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • 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
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • 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
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0045—Drying a slurry, e.g. spray drying
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/617—500-1000 m2/g

Definitions

  • the present invention relates to the field of mesostructured aluminosilicate materials with a high aluminium content. It also relates to the preparation of said materials which are obtained using the “aerosol” synthesis technique.
  • the structural and textural properties of the materials of the invention and their acid-base properties render them particularly suitable for applications in the refining and petrochemicals fields.
  • Novel synthesis strategies for producing materials with a porosity which is well defined over a very broad range, from microporous materials to macroporous materials via materials with a hierarchical porosity, i.e. with pores of various sizes, have been under development in the scientific community since the middle of the 1990s (G J de A A Soler-Illia, C Sanchez, B Lebeau, J Patarin, Chem Rev 2002, 102, 4093). Materials are obtained in which the pore size is controlled.
  • This cooperative self-organization phenomenon governed, inter alia, by the concentration of the template may be induced by progressive evaporation of a solution of reagents in which the concentration of the template is lower than the critical micellar concentration, which leads either to the formation of mesostructured films in the case of deposition onto a substrate (dip-coating) or to the formation of a mesostructured powder when the solution is atomized (aerosol technique).
  • concentration of the template is lower than the critical micellar concentration
  • 6,387,453 discloses the formation of mesostructured organic-inorganic hybrid films using the dip coating technique, the same authors having also used the aerosol technique to produce purely silicic mesostructured materials (C J Brinker, Y Lu, A Sellinger, H Fan, Adv Mater 1999, 11, 7). The pores are then released by eliminating the surfactant, this being carried out conventionally by chemical extraction or by heat treatment.
  • mesostructured materials have been developed using the different natures of the inorganic precursors and the template employed as well as the operating conditions imposed.
  • the M41S class initially developed by Mobil J S Beck, J C Vartuli, W J Roth, M E Leonowicz, C T Kresge, K D Schmitt, C T-W Chu, D H Olson, E W Sheppard, S B McCullen, J B Higgins, J L Schlenker, J Am Chem Soc, 1992, 114, 27, 10834) constituted by mesoporous materials obtained using ionic surfactants such as quaternary ammonium salts, having a generally hexagonal, cubic or lamellar structure, pores of uniform size in the range 1.5 to 10 nm and amorphous walls with a thickness of the order of 1 to 2 nm, has been widely studied.
  • ionic surfactants such as quaternary ammonium salts
  • incorporation of elemental aluminium into the amorphous silicic framework by direct synthesis or by post-synthesis processes have been particularly regarded, the aluminosilicate materials obtained having a Si/Al molar ratio in the range 1 to 1000 (S Kawi, S C Chen, Stud Surf Sci Catal 2000, 129, 227; S Kawi, S C Shen, Stud Surf Sci Catal 2000, 129, 219; R Mokaya, W Jones, Chem Commun 1997, 2185).
  • the materials thus defined are not obtained by progressive concentration of inorganic precursors and the template in an aqueous solution in which they are present, but are conventionally obtained by direct precipitation in an aqueous solvent or in high polarity solvents by adjusting the value of the critical micellar concentration of the template. Further, synthesis of such materials obtained by precipitation necessitates a step for autoclave ageing and not all of the reagents are integrated into the products in stoichiometric quantities as they can be found in the supernatant.
  • synthesis methods may take place in an acidic medium (pH approx 1) (International patent application WO-A-99/37705) or in a neutral medium (WO-A-96/39357), the nature of the template used also playing a major role.
  • the elementary particles obtained do not have a regular form and are generally characterized by dimensions of over 500 nm.
  • the mesostructured aluminosilicate materials obtained have enhanced hydrothermal stability properties compared with their homologues synthesized using other templates, their acid-basic properties remaining very similar (1 ⁇ Si/Al ⁇ 1000).
  • the invention concerns a mesostructured aluminosilicate material constituted by at least two spherical elementary particles, each of said spherical particles being constituted by a matrix based on silicon oxide and aluminium oxide, having a pore size in the range 1.5 to 30 nm, a Si/Al molar ratio of at least 1, having amorphous walls with a thickness in the range 1 to 20 nm, said spherical elementary particles having a maximum diameter of 10 ⁇ m.
  • the material of the invention has a high aluminium content and the Si/Al molar ratio is preferably in the range 1 to 10.
  • the present invention also concerns a process for preparing the material of the invention: it is obtained by interacting at least one ionic or non ionic surfactant with at least one aluminic precursor and at least one silicic precursor, preferably in an acidic medium, the ordered structure of the material following on from micellization or self-organization by evaporation induced by the aerosol technique.
  • the aluminosilicate material of the invention is a mesostructured material constituted by spherical elementary particles, each of said particles being constituted by a matrix based on silicon oxide and aluminium oxide.
  • Said matrix is mesostructured and has amorphous walls with a thickness in the range 1 to 20 nm, a uniform pore size in the range 1.5 to 30 nm and with a molar ratio Si/Al of at least 1.
  • Said spherical elementary particles advantageously have a diameter in the range 50 nm to 10 ⁇ m, preferably in the range 50 to 300 nm, the limited size of said particles and their perfectly spherical form allowing better diffusion of compounds when using the material of the invention as a catalyst or adsorbant for applications in the field of refining and petrochemistry, compared with known prior art materials in the form of elementary particles with a non homogeneous shape, i.e. irregular particles, and with a dimension which is generally over 500 nm.
  • each of said particles of the material of the invention advantageously has a Si/Al molar ratio in the range 1 to 10, more advantageously in the range 1 to 5: the material of the invention has a high aluminium content, which endows the material of the invention with advantageous acid-base properties for catalysis applications.
  • the material of the invention is also particularly advantageous for the organized porosity it has on the mesopore scale.
  • the present invention provides a mesostructured aluminosilicate material constituted by at least two spherical elementary particles, each of said spherical particles being constituted by a matrix based on silicon oxide and aluminium oxide, having a pore size in the range 1.5 to 30 nm, a Si/Al molar ratio of at least 1, having amorphous walls with a thickness in the range 1 to 20 nm, said spherical elementary particles having a maximum diameter of 10 ⁇ m.
  • the matrix based on silicon oxide and aluminium oxide constituting each of said spherical particles of the aluminosilicate material of the invention advantageously has a high aluminium content: the Si/Al molar ratio is preferably in the range 1 to 10, and more preferably in the range 1 to 5.
  • the term “mesostructured material” as used in the present invention means a material having organized porosity on the mesopore scale in each of said spherical particles, i.e. an organized porosity on the scale of pores having a uniform dimension in the range 1.5 to 30 nm, preferably in the range 1.5 to 10 nm, distributed homogeneously and in a regular manner in each of said particles (mesostructure of material).
  • the material located between the mesopores of each of said spherical particles of the material of the invention is amorphous and in the form of walls the thickness of which is in the range 1 to 20 nm.
  • the thickness of the walls corresponds to the distance separating one pore from another pore.
  • the maximum diameter of said spherical elementary particles constituting the material of the invention is 10 ⁇ m, preferably in the range 50 nm to 10 ⁇ m, and more advantageously in the range 50 to 300 nm. More precisely, said particles are present in the material of the invention in the form of aggregates.
  • the material of the invention advantageously has a specific surface area in the range 100 to 1200 m 2 /g, more advantageously in the range 300 to 1000 m 2 /g.
  • the present invention also concerns the preparation of the material of the invention.
  • Said process comprises a) mixing, in solution, at least one surfactant, at least one aluminic precursor and at least one silicic precursor; b) atomizing by aerosol the solution obtained in a) to produce spherical droplets with a diameter of less than 200 ⁇ m; c) drying said droplets and d) eliminating said surfactant to obtain a material with a mesostructured porosity.
  • the silicic and aluminic precursors used in step a) of the process of the invention are inorganic oxide precursors that are well known to the skilled person.
  • the silicic precursor is obtained from any source of silicon and advantageously from a sodium silicate precursor with formula SiO 2 , NaOH, from a chlorine-containing precursor with formula SiCl 4 , from an organometallic precursor with formula Si(OR) 4 in which R ⁇ H, methyl, ethyl or from a chloroalkoxide precursor with formula Si(OR) 4-x Cl x in which R ⁇ H, methyl, ethyl, x being in the range 0 to 4.
  • the silicic precursor may also advantageously be an organometallic precursor with formula Si(OR) 4-x R′ x in which R ⁇ H, methyl, ethyl and R′ is an alkyl chain or a functionalized alkyl chain, for example a thiol, amino, ⁇ -diketone or sulphonic acid group, x being in the range 0 to 4.
  • the aluminic precursor is advantageously an inorganic aluminium salt with formula ALX 3 , X being a halogen or the NO 3 group.
  • X is chlorine.
  • the aluminic precursor may also be an aluminium oxide or hydroxide.
  • the surfactant used to prepare the mixture of step b) of the preparation process of the invention is an ionic or non ionic surfactant or a mixture of the two.
  • the ionic surfactant is selected from phosphonium or ammonium ions, and more preferably from quaternary ammonium salts such as cetyltrimethyl ammonium bromide (CTAB).
  • CTAB cetyltrimethyl ammonium bromide
  • the non ionic surfactant may be any copolymer having at least two portions with different polarities endowing them with amphiphilic macromolecular properties.
  • a block copolymer constituted by poly (alkylene oxide) chains is used.
  • Said block copolymer is preferably a block copolymer having two, three of four blocks, each block being constituted by one poly(alkylene oxide) chain.
  • one of the blocks is constituted by a poly(alkylene oxide) chain which is hydrophilic in nature and the other block is constituted by a poly(alkylene oxide) chain which is hydrophobic in nature.
  • two of the blocks are constituted by a poly(alkylene oxide) chain which is hydrophilic in nature while the other block, located between two blocks with hydrophilic portions, is constituted by a poly(alkylene oxide) chain which is hydrophobic in nature.
  • the chains of poly(alkylene oxide) of hydrophilic nature are chains of poly(ethylene oxide), (PEO) x and (PEO) z
  • the poly(alkylene oxide) chains which are hydrophobic in nature are chains of poly (propylene oxide), (PPO) y , chains of poly(butylene oxide) or mixed chains, each chain of which is a mixture of several alkylene oxide monomers.
  • a compound with formula (PEO) x (PPO) y (PEO) z is used in which x is in the range 5 to 106, y is in the range 33 to 70 and z is in the range 5 to 106.
  • the values of x and z are identical.
  • non ionic surfactants known as Pluronic (BASF), Tetronic (BASF), Triton (Sigma), Tergitol (UnionCarbide), Brij (Aldrich) can be used as non ionic surfactants in step a) of the preparation process of the invention.
  • Pluronic BASF
  • Tetronic BASF
  • Triton Sigma
  • Tergitol UnionCarbide
  • Brij Aldrich
  • two of the blocks are constituted by a poly(alkylene oxide) chain which is hydrophilic in nature and the two other blocks are constituted by a poly(alkylene oxide) chain which is hydrophobic in nature.
  • the solution into which the following are mixed: at least one silicic precursor, at least one aluminic precursor and at least one surfactant in accordance with step a) of the preparation process of the invention, may be acidic, neutral or basic.
  • said solution is acidic and has a maximum pH of 2, more preferably in the range 0 to 2.
  • acids used to obtain an acidic solution with a maximum pH of 2 are hydrochloric acid, sulphuric acid and nitric acid.
  • Said solution may be aqueous or it may be a water-organic solvent mixture, the organic solvent preferably being a polar solvent, in particular an alcohol, preferably ethanol.
  • Said solution may also be practically organic, preferably practically alcoholic, the quantity of water being such that hydrolysis of the inorganic precursors is ensured (stoichiometric quantity). More preferably, said solution in which the following are mixed: at least one silicic precursor, at least one aluminic precursor and at least one surfactant is a hydro-organic acid mixture, more preferably an acidic water-alcohol mixture.
  • the concentrations of silicic and aluminic precursors are defined by the molar ratio Si/Al, this being at least equal to 1, preferably in the range 1 to 1000, and more preferably in the range 1 to 10 and highly preferably in the range 1 to 5.
  • the initial concentration of surfactant introduced into the mixture of step a) of the preparation process of the invention is defined by c 0 which is defined with respect to the critical micellar concentration (c mc ) which is well known to the skilled person.
  • the c mc is the limiting concentration beyond which self-arrangement of the molecules of surfactant in the solution occurs.
  • the concentration c 0 may be less than, equal to or more than c mc , preferably less than c mc .
  • the concentration c 0 is less than the c mc and said solution in step a) of the preparation process of the invention is an acidic water-alcohol acidic mixture.
  • the step for atomizing a mixture in step b) of the preparation process of the invention produces spherical droplets with a diameter which is preferably in the range 2 to 200 ⁇ m.
  • the size distribution of said droplets is of the log normal type.
  • the aerosol generator used is a commercial model 3078 apparatus supplied by TSI.
  • the solution is atomized into a chamber into which a vector gas is sent, an O 2 /N 2 mixture (dry air), at a pressure P of 1.5 bars.
  • step c) of the preparation process of the invention said droplets are dried.
  • Drying is carried out by transporting said droplets via the vector gas, the O 2 /N 2 mixture, in glass tubes, which results in progressive evaporation of the solution, for example of the hydro-organic acid solution, and the production of spherical elementary particles. Drying is completed by passing said particles into an oven the temperature of which can be adjusted, usually between temperatures of 50° C. to 600° C. and preferably 80° C. to 400° C., the residence time for said particles in the oven being of the order of 3 to 4 seconds. The particles are then harvested in a filter and constitute the material of the invention. A pump placed at the end of the circuit routes the species into the experimental aerosol device.
  • step a) of the preparation process of the invention is a water-organic solvent mixture, preferably acidic
  • the concentration of surfactant at the start of mesostructuring of the matrix is less than the critical micellar concentration so that evaporation of said hydro-organic solution, preferably acidic, during step b) of the preparation process of the invention using the aerosol technique induces a phenomenon of micellization or self-organization leading to mesostructuring of the matrix of material of the invention.
  • mesostructuring of the matrix of the material of the invention prepared using the process described above follows progressive concentration of the silicic precursor in each droplet, of the aluminic precursor, and of the surfactant, until a concentration of surfactant c>c mc results from evaporation of the hydro-organic solution, preferably acidic.
  • the aerosol technique is particularly advantageous for carrying out step b) of the preparation process of the invention to constrain the reagents present in the initial solution to interact together, with no possible loss of material apart from the solvents, the totality of the aluminium and silicon elements initially present then being perfectly preserved throughout the process of the invention instead of being eliminated during the filtering steps and washes encountered in conventional synthesis processes known to the skilled person.
  • Elimination of the surfactant in step d) of the preparation process of the invention to obtain the material of the invention with a mesostructured porosity is advantageously carried out by chemical extraction or heat treatment, preferably by calcining in air within a temperature range of 300° C. to 1000° C. and more precisely in a range of 500° C. to 600° C. for a period of 1 to 24 hours, preferably for a period of 2 to 6 hours.
  • the mesostructured aluminosilicate material with a high aluminium content of the present invention may be obtained in the form of powder, beads, pellets, granules or extrudates, the forming operations being carried out using conventional techniques which are known to the skilled person.
  • the mesostructured aluminosilicate material of the invention is obtained in the form of a powder which is constituted by spherical elementary particles having a maximum diameter of 10 ⁇ m, preferably in the range 50 to 300 nm, which facilitates any diffusion of the compounds in the case of the use of a material of the invention as a catalyst or adsorbant in refining or petrochemicals applications.
  • the mesostructured aluminosilicate material of the invention is characterized using several analytical techniques, in particular by small angle X ray diffraction (small angle XRD), the nitrogen adsorption isotherm, transmission electron microscopy (TEM) and X ray fluorescence elementary analysis.
  • Small angle X ray diffraction values of 2 ⁇ in the range 0.5° to 3° can be used to characterize the periodicity on a nanometric scale generated by the organized mesoporosity of the mesostructured matrix of the material of the invention.
  • X ray analysis is carried out on powder with a diffractometer operating in reflection equipped with a back monochromator using the copper radiation line (wavelength 1.5406 ⁇ ).
  • Nitrogen adsorption isothermal analysis corresponding to the physical adsorption of nitrogen molecules in the pores of the material on progressively increasing the pressure at constant temperature provides information regarding the textural characteristics which are peculiar to the material of the invention. In particular, it provides access to the specific surface area and to the mesoporous distribution of the material.
  • specific surface area means the BET specific surface area (S BET in m 2 /g) determined by nitrogen adsorption in accordance with American standard ASTM D 3663-78 established using the BRUNAUER-EMMETT-TELLER method described in the periodical “The Journal of the American Society”, 60, 309, (1938).
  • the pore distribution representative of a population of mesopores centered in a range of 1.5 to 50 nm is determined using the Barrett-Joyner-Halenda (BJH) model.
  • BJH Barrett-Joyner-Halenda
  • the nitrogen adsorption-desorption isotherm using the BJH model is described in the periodical “The Journal of the American Society”, 73, 373 (1951) written by E P Barrett, L G Joyner and P P Halenda.
  • the mesopore diameter ⁇ in a given mesostructured matrix corresponds to the mean diameter for nitrogen desorption defined as a diameter such that all pores with less than that diameter constitute 50% of the pore volume (Vp) measured on the desorption arm of the nitrogen isotherm.
  • the shape of the nitrogen adsorption isotherm and the hysteresis loop provides information regarding the nature of the microporosity.
  • the nitrogen adsorption isotherm of a mesostructured aluminosilicate material of the invention using a particular block copolymer, poly(ethylene oxide) 20 -poly(propylene oxide) 70 -poly(ethylene oxide) 20 (PEO 20 -PPO 70 -PEO 20 or Pluronic 123, P123) has a type IV isotherm and a type H1 hysteresis loop, the associated pore distribution curve being representative of a population of mesopores with a uniform size centered in a range of 1.5 to 30 nm.
  • TEM Transmission electron microscope analysis
  • the morphology and dimensional distribution of the elementary particles were established from analysis of the images obtained by SEM (scanning electron microscopy).
  • the structure of the mesostructured matrix constituting each of the particles of the material of the invention may be cubic, vermicular or hexagonal depending on the nature of the support selected as the template.
  • a mesostructured aluminosilicate material obtained as described above using a particular block copolymer, poly(ethylene oxide) 20 -poly(propylene oxide) 70 -poly(ethylene oxide) 20 (PEO 20 -PPO 70 -PEO 20 or Pluronic 123, P123) has a vermicular structure.
  • the present invention concerns the use of a mesostructured aluminosilicate material of the invention as an adsorbant for controlling pollution or as a molecular sieve for separation.
  • the present invention thus provides an adsorbant comprising the mesostructured aluminosilicate material of the invention. It is also advantageously used as an acidic solid to catalyze reactions, for example those occurring in the refining and petrochemistry fields.
  • the mesostructured aluminosilicate material of the invention When used as a catalyst, said material may be associated with an inorganic matrix, which may be inert or catalytically active, and a metallic phase.
  • the inorganic matrix may simply be present as a binder to keep together the particles of said material in the various known forms for catalysts (extrudates, pellets, beads, powder) or it may be added as a diluent to impose a degree of conversion on the process which would otherwise run away, leading to clogging of the catalyst due to the formation of too large an amount of coke.
  • Typical inorganic matrices are support materials for catalysts such as the various forms of silica, alumina, silica-alumina, magnesia, zirconia, titanium and boron oxides, aluminium, titanium or zirconium phosphates, clays such as kaolin, bentonite, montmorillonite, sepiolite, attapulgite, Fuller's earth, synthetic porous materials such as SiO 2 —Al 2 O 3 , SiO 2 —ZrO 2 , SiO 2 —ThO 2 , SiO 2 —BeO, SiO 2 —TiO 2 or any combination of these compounds.
  • catalysts such as the various forms of silica, alumina, silica-alumina, magnesia, zirconia, titanium and boron oxides, aluminium, titanium or zirconium phosphates, clays such as kaolin, bentonite, montmorillonite, sepiolite, attapulgit
  • the inorganic matrix may be a mixture of different compounds, in particular of an inert phase and an active phase.
  • Said material of the present invention may also be associated with at least one zeolite and may act as the principal active phase or as an additive.
  • the metallic phase may be introduced integrally onto said material of the invention.
  • cations or oxides selected from the following elements: Cu, Ag, Ga, Mg, Ca, Sr, Zn, Cd, B, Al, Sn, Pb, V, P, Sb, Cr, Mo, W, Mn, Re, Fe, Co, Ni, Pt, Pd, Ru, Rh, Os, Ir and any other element from the periodic table.
  • the catalytic compositions comprising the material of the present invention are generally suitable for carrying out the principal processes for hydrocarbon transformation and organic compound synthesis reactions.
  • the catalytic compositions comprising the material of the invention advantageously have applications in the reactions of isomerization, transalkylation and dismutation, alkylation and dealkylation, hydration and dehydration, oligomerization and polymerization, cyclization, aromatization, cracking, reforming, hydrogenation and dehydrogenation, oxidation, halogenation, hydrocracking, hydroconversion, hydrotreatment, hydrodesulphurization and hydrodenitrogenation, catalytic elimination of oxides of nitrogen, said reaction involving feeds comprising saturated and unsaturated aliphatic hydrocarbons, aromatic hydrocarbons, organic oxygen-containing compounds and organic compounds containing nitrogen and/or sulphur as well as organic compounds containing other functional groups.
  • the temperature of the drying oven was fixed at 350° C.
  • the solid was characterized by small angle XRD ( FIG. 1 ), by the nitrogen adsorption isotherm ( FIG. 2 : the indication P0 shown along the abscissa is the saturated vapour pressure), by TEM ( FIG. 3 ) and by X ray fluorescence.
  • TEM analysis showed that the final material had an organized mesoporosity characterized by a vermicular structure.
  • Small angle XRD showed a correlation peak at an angle 20 of 2.4.
  • a SEM image of the spherical elementary particles obtained indicated that the particle size was characterized by a diameter of 50 to 700 nm, with a particle size distribution being centred around 300 nm.
  • the solid was characterized by small angle XRD ( FIG. 4 ), by the nitrogen adsorption isotherm ( FIG. 5 : the indication P0 shown along the abscissa is the saturated vapour pressure), by TEM ( FIG. 6 ) and by X ray fluorescence.
  • TEM analysis showed that the final material had an organized mesoporosity characterized by a vermicular structure.
  • Small angle XRD showed a correlation peak at an angle 2 ⁇ of 0.72.
  • a SEM image of the spherical elementary particles obtained indicated that the particle size was characterized by a diameter of 50 to 700 nm, with a particle size distribution being centred around 300 nm.
  • the temperature of the drying oven was fixed at 350° C.
  • the solid was characterized by small angle XRD ( FIG. 7 ), by the nitrogen adsorption isotherm ( FIG. 8 : the indication P0 shown along the abscissa is the saturated vapour pressure), by TEM and by X ray fluorescence.
  • TEM analysis showed that the final material had an organized mesoporosity characterized by a vermicular structure.
  • Small angle XRD showed a correlation peak at an angle 2 ⁇ of 0.72.
  • a SEM image of the spherical elementary particles obtained indicated that the particle size was characterized by a diameter of 50 to 700 nm, with a particle size distribution being centred around 300 nm.

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US11/159,384 2003-10-10 2005-06-23 Mesostructured aluminosilicate material Abandoned US20060292054A1 (en)

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US20090029847A1 (en) * 2005-06-02 2009-01-29 Patrick Euzen Mesostructured material with a high aluminium content
WO2009050196A1 (fr) * 2007-10-18 2009-04-23 Commissariat A L'energie Atomique Procédé de préparation d'un géopolymère a porosité contrôlée, le géopolymère ainsi obtenu et ses differentes applications
US20100140138A1 (en) * 2006-11-23 2010-06-10 Alexandra Chaumonnot Catalyst based on a material with a hierarchical porosity comprising silicon, and a process for hydrocracking/hydroconversion and hydrotreatment of hydrocarbon feeds
US20100297002A1 (en) * 2007-09-07 2010-11-25 Ifp Crystallized silicon-containing material with hierarchical and organized porosity
US20100301263A1 (en) * 2006-10-10 2010-12-02 Choong-Kee Seong Slurry composition for a chemical mechanical polishing process and method of manufacturing a semiconductor device using the slurry composition
US20110073522A1 (en) * 2008-05-28 2011-03-31 IFP Energies Nouvelles Catalyst based on an amorphous material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US20110105300A1 (en) * 2008-03-31 2011-05-05 IFP Energies Nouvelles Mesostructured aluminosilicate material made of spherical particles of specific size
US20110111232A1 (en) * 2008-03-31 2011-05-12 Alexandra Chaumonnot Mesostructured material having a high aluminium content and consisting of spherical particles of specific size
US20110124936A1 (en) * 2008-05-28 2011-05-26 IFP Energies Nouvelles Procede doligomerisation des olefins using legeres utilisant un catalyseur a base d'un materiau amorphe a porosite hierarchisee
US20110155641A1 (en) * 2008-05-28 2011-06-30 IFP Energies Nouvelles Catalyst based on a crystalline material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US20110172482A1 (en) * 2008-05-28 2011-07-14 IFP Energies Nouvelles Catalyst based on a crystallized material with hierarchized and organized porosity and its use in oligomerization of light olefins
US20110293941A1 (en) * 2008-03-31 2011-12-01 IFP Energies Nouvelles Inorganic material made of spherical particles of specific size and having metallic nanoparticles trapped in a mesostructured matrix
WO2015191817A1 (fr) * 2014-06-12 2015-12-17 Arizona Board Of Regents On Behalf Of Arizona State University Agrégats géopolymères
US9242900B2 (en) 2009-12-01 2016-01-26 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Porous geopolymer materials
US9296654B2 (en) 2011-09-21 2016-03-29 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Geopolymer resin materials, geopolymer materials, and materials produced thereby
US9308511B2 (en) 2009-10-14 2016-04-12 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Fabricating porous materials using thixotropic gels
US9365691B2 (en) 2010-08-06 2016-06-14 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Fabricating porous materials using intrepenetrating inorganic-organic composite gels
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FR3087358A1 (fr) * 2018-10-23 2020-04-24 IFP Energies Nouvelles Materiaux aluminosilicates mesostructures utilises comme adsorbants dans les pompes a chaleur a adsorption
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US20060030477A1 (en) * 2004-06-24 2006-02-09 Alexandra Chaumonnot Material with a hierarchical porosity comprising silicon
US7994085B2 (en) 2004-06-24 2011-08-09 IFP Energies Nouvelles Material with a hierarchical porosity comprising silicon
US20060293169A1 (en) * 2005-02-09 2006-12-28 General Electric Company Molecular structures for gas sensing and devices and methods therewith
US20090029847A1 (en) * 2005-06-02 2009-01-29 Patrick Euzen Mesostructured material with a high aluminium content
US7807598B2 (en) 2005-06-02 2010-10-05 IFP Energies Nouvelles Mesostructured material with a high aluminum content
US20100301263A1 (en) * 2006-10-10 2010-12-02 Choong-Kee Seong Slurry composition for a chemical mechanical polishing process and method of manufacturing a semiconductor device using the slurry composition
US20100140138A1 (en) * 2006-11-23 2010-06-10 Alexandra Chaumonnot Catalyst based on a material with a hierarchical porosity comprising silicon, and a process for hydrocracking/hydroconversion and hydrotreatment of hydrocarbon feeds
US8821714B2 (en) 2006-11-23 2014-09-02 IFP Energies Nouvelles Catalyst based on a material with a hierarchical porosity comprising silicon, and a process for hydrocracking/hydroconversion and hydrotreatment of hydrocarbon feeds
US8623508B2 (en) 2007-09-07 2014-01-07 Ifp Crystallized silicon-containing material with hierarchical and organized porosity
US20100297002A1 (en) * 2007-09-07 2010-11-25 Ifp Crystallized silicon-containing material with hierarchical and organized porosity
FR2922543A1 (fr) * 2007-10-18 2009-04-24 Commissariat Energie Atomique Procede de preparation d'un geopolymere a porosite controlee, le geopolymere ainsi obtenu et ses differentes applications
US20100222204A1 (en) * 2007-10-18 2010-09-02 Fabien Frizon Method of preparing a controlled porosity geopolymer, the resulting geopolymer and the various applications thereof
WO2009050196A1 (fr) * 2007-10-18 2009-04-23 Commissariat A L'energie Atomique Procédé de préparation d'un géopolymère a porosité contrôlée, le géopolymère ainsi obtenu et ses differentes applications
US20110105300A1 (en) * 2008-03-31 2011-05-05 IFP Energies Nouvelles Mesostructured aluminosilicate material made of spherical particles of specific size
US20110111232A1 (en) * 2008-03-31 2011-05-12 Alexandra Chaumonnot Mesostructured material having a high aluminium content and consisting of spherical particles of specific size
US9079774B2 (en) * 2008-03-31 2015-07-14 IFP Energies Nouvelles Inorganic material made of spherical particles of specific size and having metallic nanoparticles trapped in a mesostructured matrix
US8568882B2 (en) * 2008-03-31 2013-10-29 IFP Energies Nouvelles Mesostructured material having a high aluminium content and consisting of spherical particles of specific size
US20110293941A1 (en) * 2008-03-31 2011-12-01 IFP Energies Nouvelles Inorganic material made of spherical particles of specific size and having metallic nanoparticles trapped in a mesostructured matrix
US8563135B2 (en) 2008-03-31 2013-10-22 IFP Energies Nouvelles Mesostructured aluminosilicate material made of spherical particles of specific size
US20110073522A1 (en) * 2008-05-28 2011-03-31 IFP Energies Nouvelles Catalyst based on an amorphous material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US20110172482A1 (en) * 2008-05-28 2011-07-14 IFP Energies Nouvelles Catalyst based on a crystallized material with hierarchized and organized porosity and its use in oligomerization of light olefins
US8715485B2 (en) 2008-05-28 2014-05-06 IFP Energies Nouvelles Catalyst based on an amorphous material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US8742193B2 (en) * 2008-05-28 2014-06-03 IFP Energies Nouvelles Process for oligomerization of light olefins using a catalyst based on an amorphous material with hierarchized and organized porosity
US8747652B2 (en) 2008-05-28 2014-06-10 IFP Energies Nouvelles Catalyst based on a crystalline material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US8785707B2 (en) 2008-05-28 2014-07-22 IFP Energies Nouvelles Catalyst based on a crystallized material with hierarchized and organized porosity and its use in oligomerization of light olefins
US20110155641A1 (en) * 2008-05-28 2011-06-30 IFP Energies Nouvelles Catalyst based on a crystalline material comprising silicon with a hierarchical and organized porosity, and an improved process for the treatment of hydrocarbon feeds
US20110124936A1 (en) * 2008-05-28 2011-05-26 IFP Energies Nouvelles Procede doligomerisation des olefins using legeres utilisant un catalyseur a base d'un materiau amorphe a porosite hierarchisee
US9308511B2 (en) 2009-10-14 2016-04-12 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Fabricating porous materials using thixotropic gels
US9242900B2 (en) 2009-12-01 2016-01-26 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Porous geopolymer materials
US9365691B2 (en) 2010-08-06 2016-06-14 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Fabricating porous materials using intrepenetrating inorganic-organic composite gels
US9656421B2 (en) 2010-12-22 2017-05-23 Centre National De La Recherche Scientifique Process for preparing a spherical material with a hierarchical porosity comprising metallic particles trapped in a mesostructured matrix
US9296654B2 (en) 2011-09-21 2016-03-29 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Geopolymer resin materials, geopolymer materials, and materials produced thereby
US9862644B2 (en) 2011-09-21 2018-01-09 Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And On Behalf Of Arizona State University Geopolymer resin materials, geopolymer materials, and materials produced thereby
US10170759B2 (en) 2013-06-21 2019-01-01 Arizona Board Of Regents On Behalf Of Arizona State University Metal oxides from acidic solutions
WO2015191817A1 (fr) * 2014-06-12 2015-12-17 Arizona Board Of Regents On Behalf Of Arizona State University Agrégats géopolymères
RU2701954C2 (ru) * 2014-06-12 2019-10-03 Аризона Борд Оф Риджентс Он Бихаф Оф Аризона Стейт Юниверсити Геополимерные агрегаты
US10926241B2 (en) 2014-06-12 2021-02-23 Arizona Board Of Regents On Behalf Of Arizona State University Carbon dioxide adsorbents
US11745163B2 (en) 2014-06-12 2023-09-05 Arizona Board Of Regents On Behalf Of Arizona State University Carbon dioxide adsorbents
US10829382B2 (en) 2017-01-20 2020-11-10 Skysong Innovations Aluminosilicate nanorods
CN116371416A (zh) * 2023-04-03 2023-07-04 安徽理工大学 一种镍-铌/凹凸棒石基有序介孔催化剂及其制备方法和应用

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EP1627852A1 (fr) 2006-02-22
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FR2872151A1 (fr) 2005-12-30
JP2006008509A (ja) 2006-01-12
EP1627852B1 (fr) 2011-10-12
CN1884073A (zh) 2006-12-27
US20090232720A1 (en) 2009-09-17
US7851320B2 (en) 2010-12-14
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