With Change Of Synthesized Zeolite Morphology Patents (Class 423/716)
  • Patent number: 7094390
    Abstract: There is provided macrostructures of porous inorganic material which can have controlled size, shape, and/or porosity and a process for preparing the macrostructures. The macrostructures comprise a three-dimension network of particles of porous inorganic materials. The process for preparing the macrostructures involves forming an admixture containing a porous organic ion exchanger and a synthesis mixture capable of forming the porous inorganic material and then converting the synthesis mixture to the porous inorganic material. After formation of the composite material, the porous organic ion exchanger can be removed from the composite material to obtain the macrostructures.
    Type: Grant
    Filed: May 13, 2005
    Date of Patent: August 22, 2006
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva, Valentin Panov Valtchev, Svetlana Ivanova Mintova
  • Patent number: 7081237
    Abstract: Process for the preparation of a crystalline solid comprising at least one zeolitic material, in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed directly to a drying stage.
    Type: Grant
    Filed: August 30, 2004
    Date of Patent: July 25, 2006
    Assignee: BASF Aktiengesellschaft
    Inventors: Ulrich Mueller, Friedrich Hill, Norbert Rieber
  • Patent number: 7067108
    Abstract: The synthesis of a crystalline material, in particular a high silica zeolite, having a chabazite-type framework is aided by the addition to the synthesis mixture of seeds of an AEI framework-type material. The chabazite-type product has a relatively small crystal size and exhibits activity and selectivity in the conversion of methanol to lower olefins, especially ethylene and propylene.
    Type: Grant
    Filed: December 20, 2004
    Date of Patent: June 27, 2006
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Machteld M. Mertens, Guang Cao, Hailian Li, Anil S. Guram, Robert J. Saxton, Mark T. Muraoka, Jeffrey C. Yoder
  • Patent number: 7014837
    Abstract: Described is a process to synthesize nano-size Zeolite A from an amorphous gel precursor which can be synthesized via reaction of NaAlO2, NaOH, and tetraethoxysilane (TEOS). Zeolite A with particle sizes of ˜150 nm was made by transformation of the amorphous precursor in (CH3)4NOH solution with Zeolite A seeding. The nano-sized Zeolite A can be part of processes for making non-phosphate detergent where the as-synthesized Zeolite A used as builders, for making thin films for separation and/or catalysis, for making secondary ordered patterns.
    Type: Grant
    Filed: September 16, 2003
    Date of Patent: March 21, 2006
    Assignees: E. I. duPont de Nemours and Company, Northeastern University, University of Connecticut
    Inventors: David Richard Corbin, Albert J. Sacco, Steven L. Suib, Qiuhua Zhang
  • Patent number: 7005118
    Abstract: This invention relates to a new composition of high surface area materials suitable for adsorption of both organic and inorganic species and as a component of catalysts useful for the transformation of hydrocarbons into a variety of products. These materials are composed by mesoporous spherical particles that have large sorption capacity, as demonstrated by the uptake of nitrogen at 78 K having a diameter of 0.1 to 1.0 microns, a mean pore diameter of 2.0 nm to 4.0 nm, a surface area of 750 to 1050 m2/g and a mean pore volume of 0.75 to 1.0 ml/g. The typical inner structure is composed of nanotubes having diameters around 3.5 nm aligned along the radius of the spherical particles, with surface areas around 1,000 m2/g, depending on the surfactant (C16H33N(CH3)3Br) to co-solvent (CnH2n+1OH, where n=2,3, or CH3COCH3) molar ratio.
    Type: Grant
    Filed: July 17, 2003
    Date of Patent: February 28, 2006
    Assignee: Instituto Mexicano del Petroleo
    Inventors: Eduardo Terres Rojas, Jose Manuel Dominguez Esquivel
  • Patent number: 6998104
    Abstract: Silicic and aluminum sources as raw materials of zeolite are mixed with carbon aerogel. The mixture is subjected to hydrothermal reaction for synthesis of zeolite, while an aqueous solution, which contains sodium hydroxide and tetrapropylammonium bromide, is being dropped to the mixture. After completion of the hydrothermal reaction, the zeolite-supporting aerogel is washed, dried and then heat-treated for oxidative extrusion of the carbon aerogel. Since the carbon aerogel is used as a template, the synthesized zeolite has the morphology that traces of spheroidal particles of the carbon aerogel remain as mesopores.
    Type: Grant
    Filed: December 8, 2004
    Date of Patent: February 14, 2006
    Assignee: Japan Science and Technology Agency
    Inventors: Yousheng Tao, Hirofumi Kanoh, Katsumi Kaneko
  • Patent number: 6951638
    Abstract: A process is described for producing synthetic zeolites with a MFI structure, a Si/Al atomic ratio from roughly 8 to 45 and very small primary crystallites, a Si source, an Al source and an organic template being reacted with one another under hydrothermal conditions, the Si/Al atomic ratio being roughly 9 to 50 and the ratio between the longest and shortest axis of the primary crystallites being roughly 1.0 to 1.5:1; the process is characterized in that the reaction is carried out in the presence of seed crystals with an average particle size from roughly 10 to 100 nm, preferably from 20 to 50 nm from an earlier batch without separation from the mother liquor. The zeolites as claimed in the invention which are characterized by the combination of the following features: (a) Si/Al atomic ratio 8 to 45:1 (b) Size of the primary crystallites roughly 0.01 to 0.05 microns; (c) Ratio between longest and shortest axis of the primary crystallites: roughly 1.0 to 1.
    Type: Grant
    Filed: October 11, 2000
    Date of Patent: October 4, 2005
    Assignee: Sud-Chemie AG
    Inventors: Götz Burgfels, Josef Schönlinner, Friedrich Schmidt
  • Patent number: 6949238
    Abstract: Novel zeolites are produced by combining a polar solute, a silicon or phosphorous source, and a structure directing agent. Surfactants and a hydrophobic solvent are added to the previously mixed three species and shaken to disperse the surfactants. The reverse microemulsion is stirred overnight, at about room temperature and then iced for five to ten minutes. A metal source is added vigorously shaken for about two minutes. The mixture is then aged for about two hours at about room temperature. A mineralizer is added and the resultant mixture aged for about two hours at about room temperature. The mixture is heated to about 180° C., for a suitable time period. The final novel product is then isolated.
    Type: Grant
    Filed: February 5, 2003
    Date of Patent: September 27, 2005
    Assignee: The Regents of the University of California
    Inventors: William Tumas, Kevin C. Ott, T. Mark McCleskey, Matthew Z. Yates, Eva R. Birnbaum
  • Patent number: 6949239
    Abstract: The invention involves a process for production of macrostructures of a microporous material. The process is characterized by the fact that seeds formed in or introduced by ion exchange or adsorption to a porous organic ion exchanger with the desired size, shape and porosity are made to grow and form a continuous structure by further deposition of inorganic material from a synthesis solution under hydrothermal conditions. The organic ion exchanger can be eliminated by chemical destruction or dissolution and, in so doing, leaves behind an inorganic microporous structure with the size and shape of the employed organic ion exchanger.
    Type: Grant
    Filed: March 5, 2003
    Date of Patent: September 27, 2005
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva, Valentin Panov Valtchev
  • Patent number: 6932959
    Abstract: There is provided macrostructures of porous inorganic material which can have controlled size, shape, and/or porosity and a process for preparing the macrostructures. The macrostructures comprise a three-dimension network of particles of porous inorganic materials. The process for preparing the macrostructures involves forming an admixture containing a porous organic ion exchanger and a synthesis mixture capable of forming a porous inorganic material and then converting the synthesis mixture to a solid porous inorganic material. After formation of the composite material, the porous organic ion exchanger can be removed from the composite material to obtain the macrostructures, either before or after the porous inorganic material is hydrothermally treated with a structure directing agent to convert at least a portion of such porous inorganic material to a crystalline molecular sieve composition. The resulting macrostructure is composed of particles of the crystalline molecular sieve composition.
    Type: Grant
    Filed: July 1, 2003
    Date of Patent: August 23, 2005
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva
  • Patent number: 6926882
    Abstract: There is provided macrostructures of porous inorganic material which can have controlled size, shape, and/or porosity and a process for preparing the macrostructures. The macrostructures comprise a three-dimension network of particles of porous inorganic materials. The process for preparing the macrostructures involves forming an admixture containing a porous organic ion exchanger and a synthesis mixture capable of forming a porous inorganic material and then converting the synthesis mixture to a solid porous inorganic material. After formation of the composite material, the porous organic ion exchanger can be removed from the composite material to obtain the macrostructures, either before or after the porous inorganic material is hydrothermally treated with a structure directing agent to convert at least a portion of such porous inorganic material to a crystalline molecular sieve composition. The resulting macrostructure is composed of particles of the crystalline molecular sieve composition.
    Type: Grant
    Filed: January 5, 2001
    Date of Patent: August 9, 2005
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva
  • Patent number: 6923949
    Abstract: Pure phase, high activity ZSM-48 crystals having a SiO2/Al2O3 ratio of less than about 150/1, substantially free from ZSM-50 and Kenyaite, and fibrous morphology crystals. The crystals may further have a specific cross morphology. A method for making such crystals using heterostructural, zeolite seeds, other than ZSM-48 and ZSM-50 seeds.
    Type: Grant
    Filed: March 5, 2004
    Date of Patent: August 2, 2005
    Assignee: ExxonMobil Research and Engineering Company
    Inventors: Wenyih F. Lai, Richard B. Saunders, Machteld M. Mertens, Johannes P. Verduijn
  • Patent number: 6908603
    Abstract: A novel method of forming ZSM-5 comprises reacting calcined kaolin microspheres with silicate and a seed solution used for forming zeolite Y under conditions of pH, temperature, and time to yield ZSM-5 crystals formed in-situ on said calcined kaolin microspheres. The reaction medium does not contain any organic templates or ZSM-5 seeding crystals.
    Type: Grant
    Filed: June 2, 2003
    Date of Patent: June 21, 2005
    Assignee: Engelhard Corporation
    Inventors: Mingting Xu, John Macaoay
  • Patent number: 6908604
    Abstract: There is provided macrostructures of porous inorganic material which can have controlled size, shape, and/or porosity and a process for preparing the macrostructures. The macrostructures comprise a three-dimension network of particles of porous inorganic materials. The process for preparing the macrostructures involves forming an admixture containing a porous organic ion exchanger and a synthesis mixture capable of forming the porous inorganic material and then converting the synthesis mixture to the porous inorganic material. After formation of the composite material, the porous organic ion exchanger can be removed from the composite material to obtain the macrostructures.
    Type: Grant
    Filed: April 5, 2002
    Date of Patent: June 21, 2005
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva, Valentin Panov Valtchev, Svetlana Ivanova Mintova
  • Patent number: 6893624
    Abstract: A porous, crystalline material is described having the framework structure of ZSM-12 and a composition involving the molar relationship: X2O3:(n)YO2 wherein X is a trivalent element, Y is a tetravalent element and n is less than 60. The material has an average crystal size of the material is less than 0.1 micron and a Diffusion Parameter for mesitylene of at least 1000×10?6 sec?1 when measured at a temperature of 100° C. and a mesitylene pressure of 2 torr.
    Type: Grant
    Filed: November 15, 2002
    Date of Patent: May 17, 2005
    Assignee: ExxonMobil Chemical Patents Inc.
    Inventors: Wenyih F. Lai, Ivy D. Johnson
  • Patent number: 6887457
    Abstract: A process for the preparation of a composition comprising a pentasil-type zeolite, which process comprises the following steps: a) hydrothermally treating an aqueous slurry comprising an aluminium source, a silicon source, a seeding material, and optionally a divalent metal source, thereby forming a pentasil-type zeolite and at least one other compound, and b) shaping the product of step a). Examples of the at least one other compound are anionic clay, cationic clay, Si—Al cogel, and (pseudo)boehmite.
    Type: Grant
    Filed: August 25, 2003
    Date of Patent: May 3, 2005
    Assignee: Akzo Nobel N.V.
    Inventors: Paul O'Connor, Dennis Stamires
  • Patent number: 6841144
    Abstract: The present invention concerns a method for the production of a titanium-containing zeolite whereby a synthesis gel is formed by combining and hydrolysing a hydrolysable silicon compound, a hydrolysable titanium compound and a basic quaternary ammonium compound in an aqueous medium, in quantities such that relative to the starting compounds the molar ratio of Si/Ti is greater than or equal to 30 and that of N/Si is 0.12 to less than 0.20, and the synthesis gel is then crystallised at a temperature of 150 ° C. to 220 ° C. for a period of less than 3 days, and a titanium-containing zeolite obtainable by this method.
    Type: Grant
    Filed: February 24, 2001
    Date of Patent: January 11, 2005
    Assignee: Degussa AG
    Inventors: Steffon Hasenzahl, Klaus Heyne, Dieter Kneitel
  • Patent number: 6835369
    Abstract: The present invention relates to new crystalline, molecular sieve CIT-6 that has the topology of zeolite beta. CIT-6 can be in an all-silica form, in a form wherein zinc is in the crystal framework, or a form containing silicon oxide and non-silicon oxides. In a preferred embodiment, CIT-6 has a crystal size of less than one micron and a water adsorption capacity of less than 0.05 g/g.
    Type: Grant
    Filed: December 2, 2002
    Date of Patent: December 28, 2004
    Assignee: California Institute of Technology
    Inventors: Takahiko Takewaki, Mark E. Davis
  • Patent number: 6827924
    Abstract: The present invention relates to the preparation of nanocrystalline zeolite beta by a modified aerogel protocol comprising four steps, namely, hydrolysis, nucleation, crystallization and supercritcal drying.
    Type: Grant
    Filed: November 29, 2002
    Date of Patent: December 7, 2004
    Assignee: Council of Scientific and Industrial Research
    Inventors: Kottapalli Koteswara Rao, Bhavnari Puma Chandra Rao, Boyapati Manoranjan Choudary, Lakshmi Kantam Mannepalli, Vijaya Raghavan Kondapuram
  • Publication number: 20040238407
    Abstract: A novel method of forming ZSM-5 comprises reacting calcined kaolin microspheres with silicate and a seed solution used for forming zeolite Y under conditions of pH, temperature, and time to yield ZSM-5 crystals formed in-situ on said calcined kaolin microspheres. The reaction medium does not contain any organic templates or ZSM-5 seeding crystals.
    Type: Application
    Filed: June 2, 2003
    Publication date: December 2, 2004
    Inventors: Mingting Xu, John Macaoay
  • Patent number: 6821503
    Abstract: Crystalline molecular sieve particles of a size suitable for use as seeds in molecular sieve manufacture are obtained by washing larger particle sized product to dislodge smaller particles from the larger.
    Type: Grant
    Filed: August 10, 2001
    Date of Patent: November 23, 2004
    Assignee: ExxonMobil Chemical Patents, Inc.
    Inventors: Johannes Petrus Verduijn, Machteld Maria Wilfried Mertens, Wilfried Jozef Mortier, Marcel Johannes Janssen, Cornelis Wilhelmus Maria Van Oorschot, David E. W. Vaughan
  • Patent number: 6805851
    Abstract: Process for the preparation of a crystalline solid comprising at least one zeolitic material, in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed directly to a drying stage.
    Type: Grant
    Filed: February 20, 2002
    Date of Patent: October 19, 2004
    Assignee: BASF Aktiengesellschaft
    Inventors: Ulrich Müller, Friedrich Hill, Norbert Rieber
  • Publication number: 20040200757
    Abstract: The present invention relates to new crystalline, molecular sieve CIT-6 that has the topology of zeolite beta. CIT-6 can be in an all-silica form, in a form wherein zinc is in the crystal framework, or a form containing silicon oxide and non-silicon oxides. In a preferred embodiment, CIT-6 has a crystal size of less than one micron and a water adsorption capacity of less than 0.05 g/g.
    Type: Application
    Filed: December 2, 2002
    Publication date: October 14, 2004
    Inventors: Takahiko Takewaki, Mark E. Davis
  • Patent number: 6793911
    Abstract: A method for making a zeolite includes impregnating a porous inorganic oxide with a liquid solution containing an inorganic micropore-forming directing agent. The amount of liquid solution is no more than about 100% of the pore volume of the porous inorganic oxide, and the concentration of the directing agent in the liquid solution ranges from 21% to about 60% by weight. The impregnated amorphous inorganic oxide is heated at a synthesis temperature of from about 50° C. to about 150° C. for a duration of time sufficient to form a zeolite-containing product. The method herein is advantageous for the transformation of a mesoporous or macroporous amorphous inorganic material to a composite structure containing the original mesoporous or macropores, but wherein at least some of the porous inorganic oxide material is converted to nanocrystalline zeolite, such as zeolite Y.
    Type: Grant
    Filed: February 5, 2002
    Date of Patent: September 21, 2004
    Assignee: ABB Lummus Global Inc.
    Inventors: Johannes Hendrik Koegler, Chuen Y. Yeh, Philip J. Angevine
  • Patent number: 6773693
    Abstract: A fine A-type zeolite particle having an average primary particle size of 0.1 &mgr;m or less and a variation coefficient of 90% or less, wherein a ratio of a peak area above a background level to all peak are in the range of 2&thgr;=20° to 40° in a powder X-ray diffraction spectrum of said fine A-type zeolite particle is 30% or more; a process for preparing the fine A-type zeolite particle, comprising reacting a silica source with an aluminum source in the presence of an organic compound having an oxygen-containing functional group and a molecular weight of 100 or more; and a detergent composition comprising a surfactant and the fine A-type zeolite particle. The fine zeolite particle is suitably used for detergent builders, water treatment agents, fillers for paper, resin fillers, oxygen-nitrogen separating agents, adsorbents, catalyst carriers, soil improvers for gardening, polishing agents, and the like.
    Type: Grant
    Filed: August 9, 2002
    Date of Patent: August 10, 2004
    Assignee: Kao Corporation
    Inventors: Hiroji Hosokawa, Kazuo Oki
  • Publication number: 20040151648
    Abstract: Novel zeolites are produced by combining a polar solute, a silicon or phosphorous source, and a structure directing agent. Surfactants and a hydrophobic solvent are added to the previously mixed three species and shaken to disperse the surfactants. The reverse microemulsion is stirred overnight, at about room temperature and then iced for five to ten minutes. A metal source is added vigorously shaken for about two minutes. The mixture is then aged for about two hours at about room temperature. A mineralizer is added and the resultant mixture aged for about two hours at about room temperature. The mixture is heated to about 180° C., for a suitable time period. The final novel product is then isolated.
    Type: Application
    Filed: February 5, 2003
    Publication date: August 5, 2004
    Applicant: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
    Inventors: William Tumas, Kevin C. Ott, T. Mark McCleskey, Matthew Z. Yates, Eva R. Birnbaum
  • Patent number: 6756029
    Abstract: A process for preparing molecular sieves of type Y faujasite structure is described, as well as pre-shaped bodies of faujasite structure type Y molecular sieves. The process comprises preparing a precursor gel from a source of silica-alumina or a source of alumina and a source of silica with a template agent at a SiO2/Al2O3 greater than 7 and suitable for forming a type Y zeolite, drying the precursor gel and contacting the dried precursor gel with steam, optionally followed by caustic washing, without the formation of crystalline phases other than type Y zeolite being observed. Advantageously, the pre-shaped bodies prepared with the precursor gel of Y zeolite, when subjected to the process of the invention, will have their outer surface covered by type Y zeolite crystals. The molecular sieves so obtained may be employed as catalysts or adsorbents in various processes of the chemical or oil industry.
    Type: Grant
    Filed: June 7, 2002
    Date of Patent: June 29, 2004
    Assignees: Petroleo Brasileiro S.A.-Petrobras, Akzo Nobel N.V.
    Inventors: Yiu Lau Lam, Alvaro Saavedra, Alexandre de Figueiredo Costa, Anselmo da Silva Santos, Gustavo Torres Moure, Rodolfo Eugenio Roncolatto, Dennis Stamires, Paul O'Connor
  • Patent number: 6746660
    Abstract: A process for producing ultra-fine zeolite nanocrystals and their aggregates having an intracrystalline void within 1˜10 nanometers in size that comprises at least as follows: preparing a transparent silicate-containing aqueous solution, with optional elements as Aluminum, Titanium and organic template molecules, known to produce zeolite; heating the solution under a temperature of 25°˜100° C. for a certain period of time while keeping the solution still in a transparent state without forming colloidal zeolite; adding an anionic surfactant to precipitate the inorganic components; forming the dried inorganic-organic hybrid precipitate into a desired shape and then heating the shaped body with steam under a temperature of 100°˜200° C.
    Type: Grant
    Filed: December 11, 2002
    Date of Patent: June 8, 2004
    Assignee: National Central University
    Inventors: Anthony Chiang, Ching Chuan Chen, Sajo P. Naik
  • Publication number: 20040105814
    Abstract: The present invention relates to the preparation of nanocrystalline zeolite beta by a modified aerogel protocol comprising four steps, namely, hydrolysis, nucleation, crystallization and supercritcal drying.
    Type: Application
    Filed: November 29, 2002
    Publication date: June 3, 2004
    Inventors: Kottapalli Koteswara Rao, Bhavnari Puma Chandra Rao, Boyapati Manoranjan Choudary, Lakshmi Kantam Mannepalli, Vijaya Raghavan Kondapuram
  • Patent number: 6709644
    Abstract: The present invention relates to zeolites having the crystal structure of chabazite (CHA) and having small crystallite size, to processes using the small crystallite CHA as a catalyst, and to gas separation processes using the small crystallite CHA.
    Type: Grant
    Filed: August 30, 2001
    Date of Patent: March 23, 2004
    Assignee: Chevron U.S.A. Inc.
    Inventors: Stacey I. Zones, Lun-Teh Yuen, Stephen J. Miller
  • Publication number: 20040045872
    Abstract: There is provided macrostructures of porous inorganic material which can have controlled size, shape, and/or porosity and a process for preparing the macrostructures. The macrostructures comprise a three-dimension network of particles of porous inorganic materials. The process for preparing the macrostructures involves forming an admixture containing a porous organic ion exchanger and a synthesis mixture capable of forming a porous inorganic material and then converting the synthesis mixture to a solid porous inorganic material. After formation of the composite material, the porous organic ion exchanger can be removed from the composite material to obtain the macrostructures, either before or after the porous inorganic material is hydrothermally treated with a structure directing agent to convert at least a portion of such porous inorganic material to a crystalline molecular sieve composition. The resulting macrostructure is composed of particles of the crystalline molecular sieve composition.
    Type: Application
    Filed: July 1, 2003
    Publication date: March 11, 2004
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva-Jivkova
  • Publication number: 20040047803
    Abstract: The present invention relates to a method for the preparation of zeolite particles having an average particle size of less than 1000 nm, wherein a) a solution of a silicate and/or germanate source and a base is prepared, b) a solution of an aluminate and/or gallate source and a base is prepared, and c) the solutions a) and b) are brought together, mixed and reacted, characterised in that the pH value of the solution in step a) is at least 11 and the pH value of the solution is step b) is at least 11. The invention furthermore relates to nanoscale zeolite particles obtainable by a method according to the invention and to colloidal suspensions comprising the nanoscale zeolite particles.
    Type: Application
    Filed: August 25, 2003
    Publication date: March 11, 2004
    Inventors: Valentin Panov Valtchev, Thomas Bein
  • Patent number: 6692723
    Abstract: The invention concerns a zeolite with structure type MTT comprising MTT zeolite crystals with a size of less than 5 &mgr;m, at least a portion of the MTT zeolite crystals being in the form of MTT zeolite crystal aggregates, said zeolite being characterized in that the granulometry of the aggregates is such that the dimension Dv,90 is in the range 40 nm to 100 &mgr;m. The invention also concerns the preparation of the zeolite and the use of the zeolite as a catalyst in a process for converting hydrocarbon feeds, and in particular in a process for isomerizing straight chain paraffins.
    Type: Grant
    Filed: February 21, 2001
    Date of Patent: February 17, 2004
    Assignee: Institut Francais du Petrole
    Inventors: Loïc Rouleau, Frédéric Kolenda, Eric Benazzi
  • Patent number: 6685910
    Abstract: Novel morphologies are provided for aluminosilicate zeolite ion-exchange materials useful for static water softening. The zeolites are provided in the form of large aggregates composed of submicron zeolite crystals. Rapid exchange rates, high hardness ion capacity and increased attrition resistance characterize the zeolite ion exchangers.
    Type: Grant
    Filed: December 14, 2000
    Date of Patent: February 3, 2004
    Assignee: Engelhard Corporation
    Inventors: Steven M. Kuznicki, Tadeusz W. Langner, Jacqueline S. Curran, Valerie A. Bell
  • Publication number: 20040018146
    Abstract: A fine A-type zeolite particle having an average primary particle size of 0.1 &mgr;m or less and a variation coefficient of 90% or less, wherein a ratio of a peak area above a background level to all peak are in the range of 2&thgr;=20° to 40° in a powder X-ray diffraction spectrum of said fine A-type zeolite particle is 30% or more; a process for preparing the fine A-type zeolite particle, comprising reacting a silica source with an aluminum source in the presence of an organic compound having an oxygen-containing functional group and a molecular weight of 100 or more; and a detergent composition comprising a surfactant and the fine A-type zeolite particle. The fine zeolite particle is suitably used for detergent builders, water treatment agent, fillers for paper, resin fillers, oxygen-nitrogen separating agents, adsorbents, catalyst carriers, soil improvers for gardening, polishing agents, and the like.
    Type: Application
    Filed: August 9, 2002
    Publication date: January 29, 2004
    Inventors: Hiroji Hosokawa, Kazuo Oki
  • Publication number: 20030223933
    Abstract: The invention involves a process for production of macrostructures of a microporous material. The process is characterized by the fact that seeds formed in or introduced by ion exchange or adsorption to a porous organic ion exchanger with the desired size, shape and porosity are made to grow and form a continuous structure by further deposition of inorganic material from a synthesis solution under hydrothermal conditions. The organic ion exchanger can be eliminated by chemical destruction or dissolution and, in so doing, leaves behind an inorganic microporous structure with the size and shape of the employed organic ion exchanger.
    Type: Application
    Filed: March 5, 2003
    Publication date: December 4, 2003
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva, Valentin Panov Valtchev
  • Patent number: 6656447
    Abstract: Applicants have developed a continuous process for synthesizing various molecular sieves. The process enables one to control both the particle size and particle size distribution. Any of the molecular sieves represented by the empirical formula on an anhydrous basis: rR2O:(SixAlyPz)O2, where R is at least one structure directing agent, “r”, “x”, “y” and “z” are the mole fractions of R, Si, Al and P respectively, can be prepared using this process. The process involves continuously adding separate streams comprising reactive sources of at least each framework element into a continuous crystallization reactor. Either interstage backmixing is introduced or the number of stages is adjusted in order to control particle size.
    Type: Grant
    Filed: June 28, 2001
    Date of Patent: December 2, 2003
    Assignee: UOP LLC
    Inventors: Medhat K. Tannous, Sonu Marchioretto, Lyle E. Monson
  • Patent number: 6645461
    Abstract: A process for the production of zeolites with a high Si/Al atomic ratio formed by the conversion of amorphous polysilicas (polysilacic acid) with a source of aluminum ions and optionally a template wherein the conversion occurs at a temperature of less than about 100° C., wherein ammonium hydroxide and/or an alkali metal silicate is added to the conversion solution.
    Type: Grant
    Filed: January 19, 2000
    Date of Patent: November 11, 2003
    Assignee: Sud-Chemie AG
    Inventors: Klaus K. Unger, Andreas F. K. Hahn
  • Patent number: 6641796
    Abstract: A zeolite A or an A/X mixture having an LCC>70 g liquid/100 g zeolite (hydrated) and a cold water CER>200 mg CaCO3/gram anhydrous zeolite (hydrated). The zeolite product may have a crystal size of 0.1-0.7 microns, a bulk density of 0.19-0.37 g/ml, and a median particle size of 1-5 microns. A process for making zeolite A or A/X mixtures is also claimed, including mixing a sodium silicate solution, a sodium aluminate solution, and an amorphous aluminosilicate initiator gel in a mixing vessel to create an aluminosilicate synthesis gel, and crystallizing the aluminosilicate synthesis gel to form zeolite crystals. The sodium aluminate solution may be added gradually to at least the sodium silicate solution at a rate of about 1-5% of the total batch alumina per minute, and/or a percentage of the total batch alumina may be added as alumina trihydrate (ATH) powder.
    Type: Grant
    Filed: March 16, 2001
    Date of Patent: November 4, 2003
    Assignee: PQ Corporation
    Inventors: Daniel J. Micco, Richard J. Hinchey
  • Patent number: 6635233
    Abstract: A CFI-type zeolite where the atomic ratio of silicon to the heteroatom is 45 or less and the long axes of the crystals are 0.7 &mgr;m or less is useful as a catalyst for conversion reaction of aromatic compounds because the zeolite has a number of active sites and small crystals.
    Type: Grant
    Filed: March 20, 2001
    Date of Patent: October 21, 2003
    Assignee: Toray Industries, Inc.
    Inventors: Hajime Kato, Masahito Yoshikawa, Kazuyoshi Iwayama, Shinichi Sakaguchi, Naoyuki Uchiyama
  • Patent number: 6632415
    Abstract: An in-extrudate reaction mixture to be effectively crystallized is effectively crystallized to produce zeolitic or non-zeolitic molecular sieves. The reaction mixture is heated within a slowly rotating, double-walled reactor vessel wherein a heated medium is conducted within a space formed between the double walls of the vessel. Thus, the reaction mixture is contacted by a uniformly heated wall while being gently tumbled at low speed. The tumbling action serves to uniformly distribute the heat within the reaction mixture without subjecting the mixture to such shearing that could damage shaped particles. A relatively high quantity of reaction mixture can be handled in that way to maximize the production volumes and reduce production costs.
    Type: Grant
    Filed: April 9, 2001
    Date of Patent: October 14, 2003
    Assignee: Chevron U.S.A. Inc.
    Inventors: Stephen Joseph Miller, Seymour Cherney
  • Patent number: 6620402
    Abstract: Method of preparing zeolite single crystals with straight mesopores by applying a synthesis gel with zeolite precursor composition within the pore system and on the surface of a particulate matrix material template of carbon comprising the steps of: providing a templating material with a diameter of 2 to 50 nanometers and a length-to-diameter aspect ratio of at least 5, applying the zeolite precursor to the surface of the templating material using sequential impregnation, subjecting the precursor composition to crystallising conditions, and isolating porous single zeolite crystals with straight mesopores by removing the matrix template material.
    Type: Grant
    Filed: July 6, 2001
    Date of Patent: September 16, 2003
    Assignee: Haldor Topsoe A.S
    Inventors: Claus J. H. Jacobsen, Iver Schmidt, Søren Dahl, Konrad Herbst, Søren Pehrson
  • Publication number: 20030147805
    Abstract: A method for making a zeolite includes impregnating a porous inorganic oxide with a liquid solution containing an inorganic micropore-forming directing agent. The amount of liquid solution is no more than about 100% of the pore volume of the porous inorganic oxide, and the concentration of the directing agent in the liquid solution ranges from about 21% to about 60% by weight. The impregnated amorphous inorganic oxide is heated at a synthesis temperature of from about 50° C. to about 150° C. for a duration of time sufficient to form a zeolite-containing product. The method herein is advantageous for the transformation of a mesoporous or macroporous amorphous inorganic material to a composite structure containing the original mesopores or macropores, but wherein at least some of the porous inorganic oxide material is converted to nanocrystalline zeolite, such as zeolite Y.
    Type: Application
    Filed: February 5, 2002
    Publication date: August 7, 2003
    Inventors: Johannes Hendrik Koegler, Chuen Y. Yeh, Philip J. Angevine
  • Patent number: 6596256
    Abstract: Low silicon sodium X zeolite containing little or no sodium A zeolite as by-product, is prepared by direct synthesis from sodium ion-containing hydrogels, the crystallization step being carried out by maintaining the hydrogels at a temperature below about 70° C., and preferably in the range of about 50 to about 70° C. for the duration of the crystallization step. Preferably, the ratios of components in the solutions used to make the hydrogel are such that in the hydrogel the silica/alumina molar ratio will be in the range of about 2.25:1 to about 2.4:1; the sodium oxide to silica molar ratio will be in the range 1.6:1 to about 1.9:1; and the water to sodium oxide molar ratio will be greater than about 60:1.
    Type: Grant
    Filed: August 28, 2000
    Date of Patent: July 22, 2003
    Assignee: The BOC Group, Inc.
    Inventors: Adeola F. Ojo, Frank R. Fitch, Martin Bülow, Craig S. Gittleman, Sudhakar R. Jale
  • Publication number: 20030127359
    Abstract: The present invention relates to new crystalline, molecular sieve CIT-6 that has the topology of zeolite beta. CIT-6 can be in an all-silica form, in a form wherein zinc is in the crystal framework, or a form containing silicon oxide and non-silicon oxides. In a preferred embodiment, CIT-6 has a crystal size of less than one micron and a water adsorption capacity of less than 0.05 g/g.
    Type: Application
    Filed: December 2, 2002
    Publication date: July 10, 2003
    Inventors: Takahiko Takewaki, Mark E. Davis
  • Publication number: 20030129128
    Abstract: The present invention provides a method for the synthesis of MeAPO molecular sieves which includes the following steps: providing a source of alumina, a source of phosphorus, water, and a template suitable for forming a MeAPO molecular sieve; providing a source of metal (Me) including metal particles, the metal particles measuring, in their largest dimension, equal to or less than five nanometers; providing a water soluble organic solvent capable of solubilizing the source of metal; forming a synthesis mixture from the source of alumina, the source of phosphorus, the water, the template, the source of metal, and the solvent; and forming a MeAPO molecular sieve from the synthesis mixture.
    Type: Application
    Filed: January 21, 2003
    Publication date: July 10, 2003
    Inventors: Karl G. Strohmaier, David E.W. Vaughan
  • Publication number: 20030103894
    Abstract: The present invention concerns a method for the production of a titanium-containing zeolite whereby a synthesis gel is formed by combining and hydrolysing a hydrolysable silicon compound, a hydrolysable titanium compound and a basic quaternary ammonium compound in an aqueous medium, in quantities such that relative to the starting compounds the molar ratio of Si/Ti is greater than or equal to 30 and that of N/Si is 0.12 to less than 0.20, and the synthesis gel is then crystallised at a temperature of 150° C. to 220 ° C. for a period of less than 3 days, and a titanium-containing zeolite obtainable by this method.
    Type: Application
    Filed: September 3, 2002
    Publication date: June 5, 2003
    Inventors: Steffon Hasenzahl, Klaus Heyne, Dieter Kneitel
  • Patent number: 6569400
    Abstract: The invention involves a process for production of macrostructures of a microporous material. The process is characterized by the fact that seeds formed in or introduced by ion exchange or adsorption to a porous organic ion exchanger with the desired size, shape and porosity are made to grow and form a continuous structure by further deposition of inorganic material from a synthesis solution under hydrothermal conditions. The organic ion exchanger can be eliminated by chemical destruction or dissolution and, in so doing, leaves behind an inorganic microporous structure with the size and shape of the employed organic ion exchanger.
    Type: Grant
    Filed: May 17, 1999
    Date of Patent: May 27, 2003
    Assignee: Exxon Mobil Chemical Patents Inc.
    Inventors: Per Johan Sterte, Lubomira Borislavova Tosheva, Valentin Panov Valtchev
  • Patent number: 6565826
    Abstract: Method of preparing zeolite single crystals comprising the step of: applying a synthesis gel with zeolite precursor composition within pore system and on surface of a particulate matrix material having a predetermined pore structure and particle size; subjecting the precursor composition to crystallising conditions; and isolating porous single crystals of the zeolite by removing the matrix material.
    Type: Grant
    Filed: December 5, 2000
    Date of Patent: May 20, 2003
    Assignee: Haldor Topsoe A/S
    Inventors: Claus J. H. Jacobsen, Jindrich Houzvicka, Iver Schmidt, Claus Madsen, Anna Carlsson
  • Patent number: 6541066
    Abstract: The invention relates to a method for applying a non-permeable, ceramic layer of a thickness of not more than about 100 &mgr;m to a ceramic or metallic body by applying a solution of one or more elastomers, which elastomers contain substantially not exclusively sulfur, carbon, hydrogen and oxygen, optionally drying, and pyrolyzing to form a porous layer and subsequently sintering at increased temperature to form a non-permeable ceramic layer.
    Type: Grant
    Filed: June 12, 2000
    Date of Patent: April 1, 2003
    Assignee: Universiteit Utrecht
    Inventor: John Wilhelm Geus