WO2020076745A1 - Particules poreuses contenant de la zéolite dotées d'une structure de pores hiérarchique - Google Patents

Particules poreuses contenant de la zéolite dotées d'une structure de pores hiérarchique Download PDF

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Publication number
WO2020076745A1
WO2020076745A1 PCT/US2019/055087 US2019055087W WO2020076745A1 WO 2020076745 A1 WO2020076745 A1 WO 2020076745A1 US 2019055087 W US2019055087 W US 2019055087W WO 2020076745 A1 WO2020076745 A1 WO 2020076745A1
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WIPO (PCT)
Prior art keywords
batch
porous zeolite
zeolite
particles
ceramic
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Ceased
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PCT/US2019/055087
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English (en)
Inventor
Samuel Morse KOCH
Michael Francis
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Saint Gobain Ceramics and Plastics Inc
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Saint Gobain Ceramics and Plastics Inc
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Publication of WO2020076745A1 publication Critical patent/WO2020076745A1/fr
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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
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04—Alumina
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/066—Zirconium or hafnium; Oxides or hydroxides 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • 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
    • 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
    • B01J35/64—Pore diameter
    • B01J35/647—2-50 nm
    • 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
    • B01J35/64—Pore diameter
    • B01J35/651—50-500 nm
    • 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
    • B01J35/66—Pore distribution
    • 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
    • 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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • 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
    • B01J2235/00—Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
    • B01J2235/15—X-ray diffraction
    • 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
    • B01J2235/00—Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
    • B01J2235/30—Scanning electron microscopy; Transmission electron microscopy
    • 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
    • B01J35/45—Nanoparticles
    • 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
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/51—Spheres

Definitions

  • each of the plurality of porous zeolite-containing particles comprises mesopores ranging about 2 to 50 nanometers in diameters and
  • FIG. 3 includes a flow chart illustrating other embodiments of a process for forming a batch of porous zeolite-containing ceramic particles with a hierarchical structure
  • FIG. 5 includes a schematic diagram of an embodiment of a porous zeolite- containing ceramic particle showing a core region and a layered region with multiple layered sections of the particle;
  • Dense, spherical zeolite-containing particles may be prepared by spray fluidization. However, such particles are prepared using a continuous spray fluidization forming process. Producing zeolite-containing particles having the various desired qualities noted above, such as, a particular porosity and with a narrow size distribution using a continuous spray fluidization forming process requires a complex manufacturing process that may include intermediate and/or post-process mechanical screening operations (i.e., cutting, grinding or filtering) to reduce and normalize the average particle size of oversized fractions of the zeolite-containing ceramic particles. These fractions may then be recycled back to the continuous process or otherwise recycled or be potentially considered as a lost material.
  • intermediate and/or post-process mechanical screening operations i.e., cutting, grinding or filtering
  • the coating fluid includes a slurry mix of zeolite and alumina.
  • the coating fluid includes a slurry mix of zeolite and suitable ceramic materials such as alumina, zirconia, titania, silica, hafnia or a combination thereof.
  • the coating fluid includes a slurry mix of zeolite and other ceramic materials.
  • the coating fluid includes a slurry mix of no greater than 90% of ceramic material, such as, no greater than 80% of ceramic material, no greater than 70% of ceramic material, no greater than 60% of ceramic material, no greater than 50% of ceramic material, no greater than 40% of ceramic material, no greater than 30% of ceramic material, no greater than 20% of ceramic material, or no greater than 10% of ceramic material.
  • the coating fluid includes a slurry mix of at least 20% of ceramic material and up to 80% of zeolite.
  • the coating fluid includes no greater than 90% of ceramic materials, and at least 10% of zeolite.
  • the coating fluid includes no greater than 80% of ceramic materials, and at least 20% of zeolite.
  • the initial particle size distribution span IPDS of the initial batch of ceramic particles is equal to (M90 -Idio)/Id 5 o, where H90 is equal to a dgo, a cumulative 90% pass particle size distribution measurement of the initial batch of ceramic particles; Id l0 is equal to a dio, a cumulative 10% pass particle size distribution measurement of the initial batch of ceramic particles; and Idso is equal to a dso, a cumulative 50% pass particle size distribution measurement of the initial batch of ceramic particles.
  • H90 is equal to a dgo
  • Id l0 is equal to a dio
  • Idso is equal to a dso, a cumulative 50% pass particle size distribution measurement of the initial batch of ceramic particles.
  • particle size distribution measurements can be determined by a particle size analyzer, for example, a Malvern Mastersizer 2000 or a
  • the first coating material composition may include a particular concentration of a material or particular concentrations of multiple materials as measured in volume percent for a total volume of the first coating fluid.
  • the layered region may have a porosity of any value between any of the minimum and maximum values noted above. It will be further appreciated that the layered region may have a porosity of any value within a range between any of the minimum and maximum values noted above. In some embodiments, the layered region 420 may have an average porosity of at least about 0.6 cc/g and not greater than about 1.9 cc/g, such as, at least about 0.9 cc/g and not greater than about 1.7 cc/g, or at least about 0.9 cc/g and not greater than about 1.5 cc/g.
  • the core region 510 may be different than the second layered section 524. According to still other embodiments, the core region 510 may have different composition than the second layered section 524. According to particular embodiments, the core region 510 and the second layered section 524 may be formed of different materials and/or different relative concentration of materials. According to yet other embodiments, the core region 510 may have a different microstructure than the second layered section 524. According to yet other embodiments, the core region 510 may have a different particle density than the second layered section 524, where the particle density is the particle mass divided by the particle volume including intraparticle porosity. According to yet other embodiments, the core region 510 may have a different porosity than the second layered section 524.
  • the second layered section 524 may be defined as having an inner surface 524 A and an outer surface 524B.
  • the inner surface 524 A of the second layered section 524 is defined as the surface closest to the first layered section 522.
  • the outer surface 524B of the second layered section 524 is defined as the surface farthest from the first layered section 522.
  • a third layer section 526 may include overlapping layers surrounding the second layered section 524.
  • the layered region may have a porosity of any value between any of the minimum and maximum values noted above. It will be further appreciated that the layered region may have a porosity of any value within a range between any of the minimum and maximum values noted above.
  • the third layer section 526 may make up a particular volume percentage of the total volume of the porous zeolite-containing ceramic particle 500.
  • the third layer section 526 may make up at least about 50 vol% of the total volume of the porous zeolite-containing ceramic particle 500, such as, at least about 55 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 60 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 65 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 70 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 75 vol of the total volume of the porous zeolite-containing ceramic particle 500, at least about 80 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 85 vol% of the total volume of the porous zeolite-containing ceramic particle 500, at least about 90 vol%
  • the third layered section composition may include, in addition to zeolite, any one of lanthanum (La), zinc (Zn), nickel (Ni), cobalt (Co), niobium (Nb), tungsten (W), magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), bismuth (Bi) or combinations thereof.
  • At least 20 samples are used to determine a statistically reliable value of Idio, Idso , 90, Pdio, and Pdso,

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé de formation de particules céramiques poreuses contenant de la zéolite, dotées d'une structure hiérarchique, comprenant l'utilisation d'un processus de formation de fluidisation par pulvérisation réalisé dans un mode par lots comprenant un ou plusieurs cycles de formation de fluidisation par pulvérisation par lots. Dans chacun des cycles de formation, un lot initial de particules céramiques est revêtu d'un mélange de suspension de zéolite et de matériaux céramiques en vue de former un lot traité de particules céramiques poreuses contenant de la zéolite. Le lot traité de particules céramiques poreuses contenant de la zéolite peut être utilisé comme lot initial dans le cycle de formation suivant. Les particules céramiques poreuses contenant de la zéolite formées par le processus de formation de fluidisation par pulvérisation peuvent comprendre des structures mésopore et macropore dans une région en couches recouvrant une région centrale de chaque particule.
PCT/US2019/055087 2018-10-12 2019-10-08 Particules poreuses contenant de la zéolite dotées d'une structure de pores hiérarchique Ceased WO2020076745A1 (fr)

Applications Claiming Priority (2)

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US201862744712P 2018-10-12 2018-10-12
US62/744,712 2018-10-12

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WO2020076745A1 true WO2020076745A1 (fr) 2020-04-16

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040009340A1 (en) * 2002-07-12 2004-01-15 Jesse Zhu Fluidization additives to fine powders
US20080213154A1 (en) * 2004-06-23 2008-09-04 Philippe Kalck Divided Solid Composition Composed of Grains Provided with Continuous Metal Deposition, Method for the Production and Use Thereof in the Form of a Catalyst
WO2017042611A1 (fr) * 2015-09-11 2017-03-16 Saint-Gobain Ceramics & Plastics, Inc. Procédé de formation de particules en céramique poreuse
US20180001301A1 (en) * 2014-12-23 2018-01-04 John F. Brody Structured Adsorbent Beds, Methods of Producing the Same and uses Thereof
WO2018026574A1 (fr) * 2016-08-01 2018-02-08 W. R. Grace & Co.-Conn. Procédé de peptisation d'alumine pour catalyseurs fluidisables
WO2018169753A1 (fr) * 2017-03-14 2018-09-20 Saint-Gobain Ceramics & Plastics, Inc. Particules céramiques poreuses et leur procédé de formation

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040009340A1 (en) * 2002-07-12 2004-01-15 Jesse Zhu Fluidization additives to fine powders
US20080213154A1 (en) * 2004-06-23 2008-09-04 Philippe Kalck Divided Solid Composition Composed of Grains Provided with Continuous Metal Deposition, Method for the Production and Use Thereof in the Form of a Catalyst
US20180001301A1 (en) * 2014-12-23 2018-01-04 John F. Brody Structured Adsorbent Beds, Methods of Producing the Same and uses Thereof
WO2017042611A1 (fr) * 2015-09-11 2017-03-16 Saint-Gobain Ceramics & Plastics, Inc. Procédé de formation de particules en céramique poreuse
WO2018026574A1 (fr) * 2016-08-01 2018-02-08 W. R. Grace & Co.-Conn. Procédé de peptisation d'alumine pour catalyseurs fluidisables
WO2018169753A1 (fr) * 2017-03-14 2018-09-20 Saint-Gobain Ceramics & Plastics, Inc. Particules céramiques poreuses et leur procédé de formation

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