By Precipitating Patents (Class 423/339)
  • Patent number: 6500870
    Abstract: A method for production of high purity silica sols comprising the steps: (a) adding a phosphonic acid-based complexing agent to the silicic acid-containing solution forming complexes with metal cations present in said solution; (b) forming in said silicic acid-containing solution a precipitation containing phosphonic acid-based complexing agent and metal cations; (c) removing the precipitation from the solution; and, (d) polymerising the silicic acid in the solution to obtain a silica sol. The invention also relates to silica sols containing at least one phosphonic acid-based complexing agent.
    Type: Grant
    Filed: November 15, 2000
    Date of Patent: December 31, 2002
    Assignee: Akzo Nobel N.V.
    Inventors: Magnus Olof Linsten, Bozena Stanislawa Tokarz, Kenneth Olof Larsson
  • Patent number: 6479036
    Abstract: Silica particles for incorporation into a dentifrice composition, preferably as a thickening agent, have a polyether glycol such as polyethylene glycol applied thereto in order to enhance dentifrice cohesion
    Type: Grant
    Filed: December 5, 2000
    Date of Patent: November 12, 2002
    Assignee: Crosfield Limited
    Inventors: Peter W Stanier, Charlotte R Evans
  • Patent number: 6468493
    Abstract: The invention relates to a novel process for the preparation of precipitated silica which can be used as a reinforcing filler for elastomers. The invention also relates to novel precipitated silicas in the form of powder, granules or, preferably, substantially spherical beads, these silicas being characterized in that they have a BET specific surface of between 185 and 250 m2/g, a CTAB specific surface of between 180 and 240 m2/g, and a pore distribution such that the pore volume V2 made up of the pores with a diameter of between 175 and 275 Å represents less than 50% of the pore volume V1 made up of the pores with diameters of less than or equal to 400 Å, a pore volume (Vd1), made up of the pores with a diameter of less than 1 &mgr;m, of greater than 1.65 cm3/g, a fineness value (F.V.) of between 70 and 100 Å, and a content of fines (&tgr;f), after deagglomerability with ultrasound, of at least 50%.
    Type: Grant
    Filed: July 23, 1999
    Date of Patent: October 22, 2002
    Assignee: Rhodia Chimie
    Inventors: Yvonick Chevallier, Philippe Cochet, Patrick Fourre
  • Patent number: 6448331
    Abstract: Disclosed is an alkoxysilane/organic polymer composition for use in producing an insulating thin film, comprising (A) a specific alkoxysilane; (B) a specific organic polymer; and (C) a solvent for alkoxysilane (A) and organic polymer (B), wherein solvent (C) comprises at least one organic solvent selected from the group consisting of amide linkage-containing organic solvents and ester linkage-containing organic solvents. Also disclosed are a silica-organic polymer composite thin film which is produced by a process comprising: forming a thin film of the composition of the present invention; subjecting the thin film to a hydrolysis and dehydration-condensation reaction with respect to the alkoxysilane thereof, to thereby cause the alkoxysilane to be gelled in the thin film; and removing the solvent remaining in the thin film by drying, and a porous silica thin film which is obtained by removing the organic polymer from the silica-organic polymer composite thin film.
    Type: Grant
    Filed: November 12, 1999
    Date of Patent: September 10, 2002
    Assignee: Asahi Kasei Kabushiki Kaisha
    Inventors: Takaaki Ioka, Tsuneaki Tanabe
  • Patent number: 6440397
    Abstract: Silica compositions for abrasive systems in dentifrice formulations are disclosed. The silica abrasive system comprises (a) silica gels having a median particle size below 7 microns, a pH of from about 6 to about 11 and powder RDA's of from 100 to about 200 and (b) silica gels or precipitates having a median particle size of 7 microns or greater and powder RDA's of from 50 to about 180. Silica (a) is preferably prepared by contacting a hydrous silica gel with an alkaline medium. Dentifrice compositions comprising the abrasive system has an RDA of 150 or less and PCR's of at least 80 and up to about 150, and an REA of less than about 30 (as measured on the IU scale).
    Type: Grant
    Filed: July 31, 2001
    Date of Patent: August 27, 2002
    Assignee: W. R. Grace & Co. -Conn.
    Inventors: Michael Bruce Thomas, Michael Vance Ernest, Sandra Joan Kempske
  • Patent number: 6432151
    Abstract: Disclosed herein is a method of preparing silica slurry for wafer polishing. This method includes pre-treating relatively inexpensive and commercially available fumed or colloidal silica particles as a seed by a settling, a crushing using a ball mill and a paint shaker, and a sonication to produce an aqueous dispersion of the silica particles. The pre-treated silica particles are then combined with tetraethylorothosilicate as a precursor, an alcohol solvent and a base, and grown to a desired size by hydrolysis and polycondensation of the precursor, tetraethylorothosilicate. Then, the alcohol solvent, in which the silica particles are grown, are displaced with water by a vacuum distillation. The resulting aqueous dispersion of the grown silica dispersion is hydrothermally treated in an autoclave. Thus, this method allows the economical preparation of the spherical silica particles having a highly uniform size and a very high purity.
    Type: Grant
    Filed: August 22, 2000
    Date of Patent: August 13, 2002
    Assignee: Korea Advanced Institute of Science and Technology
    Inventors: Jae Hyun So, Min Ho Oh, Sun Hyuck Bae, Seung Man Yang, Do Hyun Kim
  • Patent number: 6419174
    Abstract: Abrasive compositions comprised of water-insoluble abrasive polishing agents suspended in a liquid medium in combination with humectant, and methods for making same. The inventive abrasive compositions are rheologically stable, settling-resistant, and re-agglomeration resistant, even during and after transport and/or storage before end-use, such as incorporation into dentifrice formulations or other oral cleaning compositions. The high settling-resistance of the inventive abrasive composition makes it possible to avoid the need before end use for temporary stabilizers such as inorganic suspending agents (e.g., clays, fumed silicas) or organic binders (e.g., polysaccharides). Also, the abrasive compositions contain abrasive particles having improved brightness as compared to abrasive particles made via drying and dry comminution processing.
    Type: Grant
    Filed: August 18, 2000
    Date of Patent: July 16, 2002
    Assignee: J. M. Huber Corporation
    Inventors: Patrick D. McGill, Michel J. Martin, Donald M. Gury
  • Patent number: 6419891
    Abstract: This invention relates to a new synthetic crystalline material comprising acidic surface silanol groups, designated MCM-69, a method for its preparation and use thereof in catalytic conversion of organic compounds.
    Type: Grant
    Filed: October 18, 1999
    Date of Patent: July 16, 2002
    Assignee: ExxonMobil Oil Corporation
    Inventors: Carrie L. Kennedy, Gordon J. Kennedy, Stephen L. Lawton, Louis D. Rollmann, John L. Schlenker
  • Patent number: 6403059
    Abstract: Methods of making dentifrice compositions including, as a raw material ingredient thereof, abrasive compositions comprised of water-insoluble abrasive polishing agents suspended in a liquid medium in combination with humectant, and the unique dentifrice compositions made in this manner.
    Type: Grant
    Filed: August 18, 2000
    Date of Patent: June 11, 2002
    Assignee: J. M. Huber Corporation
    Inventors: Michel J. Martin, Patrick D. McGill, Donald M. Gury, Yung-Hui Huang, Minas R. Apelian
  • Patent number: 6399111
    Abstract: An amorphous silica having an RDA value of between 40 and 70, an oil absorption capacity of between 90 and 145 cc/100 g and a moisture loss of less than 7% w/w, can be incorporated at a 10% to 25% loading into a transparent toothpaste having a refractive index of below 1.445, this toothpaste having an RDA value of less than 60.
    Type: Grant
    Filed: September 14, 1999
    Date of Patent: June 4, 2002
    Assignee: Crosfield Limited
    Inventor: Peter W. Stanier
  • Patent number: 6395247
    Abstract: The precipitated silica has the following physico-chemical parameters: BET surface area (DIN 66131) in m2/g 400-600 DBP index (DIN 53601) in g/100 g 300-360 Compacted density (DIN 53194) in g/l  70-140 Grindometer value (ISO 1524) in &mgr;m 15-50 Size distribution index I <1.0 measured with a Malvern instrument Size distribution index I = d 90 - d 10 2 ⁢ d 50 This precipitated silica is prepared by milling a precipitated silica in accordance with DE-A 31 44 299 in a classifier mill or a fluidized bed counter-flow mill. A polyethylene wax emulsion may be added before the milling procedure.
    Type: Grant
    Filed: December 10, 1998
    Date of Patent: May 28, 2002
    Assignee: Degussa AG
    Inventors: Mustafa Siray, Jochen Scheffler
  • Patent number: 6395807
    Abstract: The fine spherical silica having a particle size distribution in which maximum particle diameter is 24 &mgr;m, average particle diameter is 1.7 to 7 &mgr;m, and the proportion X1 of particles having a particle diameter of 3 &mgr;m or less in the total particles is 100/D50 to (18+100/D50) wt %, and the viscosity at 50° C. of a mixture obtained by blending a maximum of 80 wt % of the fine spherical silica with a liquid epoxy resin or silicone resin at room temperature is 20 Pa·s or less is provided. The spherical silica is useful as a filler for sealing resin composition which has excellent gap permeability and seals slight gaps, between a substrate and an IC chip and has high reliability.
    Type: Grant
    Filed: April 11, 2000
    Date of Patent: May 28, 2002
    Assignee: Nippon Chemical Industrial Co., LTD
    Inventors: Yutaka Kinose, Shinsuke Miyabe, Takeshi Sakamoto
  • Patent number: 6383280
    Abstract: The precipitated silica has the following physico-chemical parameters: BET surface area (DIN 66131) in m2/g 400-600 DBP index (DIN 53601) in g/100 g 300-360 Compacted density (DIN 53194) in g/l  70-140 Grindometer value (ISO 1524) in &mgr;m 15-50 Size distribution index I <1.0 measured with a Malvern instrument Size ⁢   ⁢ distribution ⁢   ⁢ index ⁢   ⁢ I = d 90 - d 10 2 ⁢ d 50 This precipitated silica is prepared by milling a precipitated silica in accordance with DE-A 31 44 299 in a classifier mill or a fluidized bed counter-flow mill.
    Type: Grant
    Filed: April 18, 2000
    Date of Patent: May 7, 2002
    Assignee: Degussa-Huls AG
    Inventors: Mustafa Siray, Jochen Scheffler
  • Patent number: 6380265
    Abstract: A dispersion comprising fine porous inorganic oxide particles, e.g., silica gel particles, wherein the particles have a median particle size below three microns. The dispersed particles have a porosity after drying in which at least about 0.50 cc/g of pore volume is from pores having a pore size of 600 Å or less as determined by nitrogen porosimetry. Embodiments prepared from silica gel have porosity after drying in which at least about 0.7 cc/g of pore volume is from pores having a diameter of 600 Å or smaller. The particles of the dispersion also can be described as having viscosity derived pore volume of at least about 0.5 g/cc. The dispersion is prepared by forming a dispersion from inorganic oxides having sufficient rigid structure to maintain porosity after milling and drying. After the inorganic oxide is selected, it is milled to have a median particle size of 0.05 to about 3 microns.
    Type: Grant
    Filed: June 30, 1999
    Date of Patent: April 30, 2002
    Assignee: W. R. Grace & Co.-Conn.
    Inventors: James Neil Pryor, David Monroe Chapman
  • Patent number: 6342193
    Abstract: The present invention provides the amorphous silica particles having a double structure of a core of the dense amorphous silica and a shell of the bulky amorphous silica, having a volume-based median diameter of from 1 to 5 &mgr;m and containing not more than 10% by volume of fine particles having a particle diameter of not larger than 0.5 &mgr;m. The amorphous silica particles of the double structure have constant particle diameters not only in the powdery state but also in a state where they are blended in a coating material or in a resin, without developing fine particles, exhibit excellent delustering action and antiblocking action, exhibit decreased abrading property, and exhibit excellent resistance against scars or abrasion.
    Type: Grant
    Filed: May 1, 2000
    Date of Patent: January 29, 2002
    Assignee: Mizusawa Industrial Chemicals A.S.
    Inventors: Masanori Tanaka, Yuuji Washio
  • Patent number: 6334880
    Abstract: Non-spherical silica particles having nodular morphology for use as an abrasive media in chemical mechanical polishing are disclosed. Also disclosed are aqueous slurries of monodispersed non-spherical nodular shaped particles having mean effective diameters between about 100 and 300 nanometers for chemical mechanical polishing. In addition aqueous slurries for the chemical mechanical polishing and planarization of oxide dielectric, metal, and metal/metallic compound interlayers of integrated circuits are disclosed.
    Type: Grant
    Filed: December 7, 1999
    Date of Patent: January 1, 2002
    Assignee: Silbond Corporation
    Inventors: John A. Negrych, George Haag, Peter E. Rall, William J. Corbell
  • Publication number: 20010043901
    Abstract: A process for the preparation of mesostructured molecular sieve silicas from inorganic silicon precursors and polyoxyethylene oxide based polymers is described. The silicas are stable upon calcination to 600° to 800° C. The silicas are useful in refining processes.
    Type: Application
    Filed: April 13, 2001
    Publication date: November 22, 2001
    Applicant: Board of Trustees Operating Michigan State Univ.
    Inventors: Thomas J. Pinnavaia, Thomas R. Pauly, Seong-Su Kim
  • Patent number: 6312601
    Abstract: A process and system for removing heavy metals, fluoride, silica and other contaminants from large volumes of wastewater is disclosed. In the process, a wastewater stream containing the contaminant is treated with a chemical coagulant to create a particle having a diameter greater than 5 microns. Treated wastewater is passed through a microfiltration membrane which physically separates the metal contaminant particle from the wastewater. Commercially available microfiltration membranes having a pore size from 0.5 micron to 5 microns may be used. The treated wastewater flow rate through the microfiltration membranes can range from 700 gallons per square foot of membrane per day (“GFD”) to 1500 GFD. Solids are removed from the membrane surface by periodically backflushing the micro-filtration membranes and draining the filtration vessel within which the membranes are located. The dislodged solid material within the filtration vessel is flushed into a holding tank for further processing of the solids.
    Type: Grant
    Filed: August 30, 2000
    Date of Patent: November 6, 2001
    Assignee: Microbar Incorporated
    Inventors: Stephen D. Allen, Josh H. Golden
  • Patent number: 6294155
    Abstract: Silica compositions for abrasive systems in dentifrice formulations are disclosed. The silica abrasive system comprises (a) silica gels having a median particle size below 7 microns, a pH of from about 6 to about 11 and powder RDA's of from 100 to about 200 and (b) silica gels or precipitates having a median particle size of 7 microns or greater and powder RDA's of from 50 to about 180. Silica (a) is preferably prepared by contacting a hydrous silica gel with an alkaline medium. Dentifrice compositions comprising the abrasive system has an RDA of 150 or less and PCR's of at least 80 and up to about 150, and an REA of less than about 30 (as measured on the IU scale).
    Type: Grant
    Filed: April 8, 1998
    Date of Patent: September 25, 2001
    Assignee: W. R. Grace & Co. -Conn.
    Inventors: Michael Bruce Thomas, Michael Vance Ernest, Sandra Joan Kempske
  • Patent number: 6290924
    Abstract: Essentially spherical precipitated silica beads, well adapted for the reinforcement of elastomeric matrices, have a mean particle size of at least 80 &mgr;m, a BET specific surface area ranging from 60 to 130 m2/g, a fill density in packed state ranging from 0.28 to 0.37, and a total pore volume ranging from 1.6 to 3.3 cm3/g.
    Type: Grant
    Filed: April 17, 2000
    Date of Patent: September 18, 2001
    Assignee: Rhone-Poulenc Chimie
    Inventor: Yvonick Chevallier
  • Patent number: 6290933
    Abstract: A high cleaning low abrasion dentifrice containing a silica hydrogel having a mean particle size from about 5 to about 11 microns; an Einlehner hardness of from 1 to about 20; an oil absorption of about 40 to less about 100 cc/g, a BET surface area from 100 to 700 m2/g of silica, the particles having a morphology characterized by glass conchoidal fracture surfaces whereby, the dentifrice composition has a RDA of 110 to 200 and a PCR from about 150 to about 300.
    Type: Grant
    Filed: May 9, 2000
    Date of Patent: September 18, 2001
    Assignee: Colgate-Palmolive Company
    Inventors: Gary A. Durga, Michael Prencipe, Peter J. Priolo, Peter Ren
  • Publication number: 20010018038
    Abstract: The present invention relates to a process for easily and efficiently producing silica particles having a narrow particle size distribution and a high porosity from inexpensive starting materials such as sodium silicate. The silica particles of the present invention can be obtained in the form of a slurry containing them by (1) forming a slurry by mixing first particles difficultly soluble in an alkali and soluble in an acid, with an aqueous alkali silicate solution to form a first slurry containing the first particles, (2) neutralizing the first slurry with a mineral acid to prepare a second slurry containing second particles wherein silica is deposited on the first particles, and (3) adding a mineral acid to the second slurry to dissolve the first particles from the second particles, to prepare a third slurry containing silica particles.
    Type: Application
    Filed: April 12, 2001
    Publication date: August 30, 2001
    Applicant: Oji Paper Co., Ltd.
    Inventors: Masashi Matsuda, Masasuke Watanabe, Hitoshi Okada, Motohide Wada, Osamu Kitao
  • Patent number: 6268424
    Abstract: Precipitated silica having the following parameters: BET surface area 80-180 m2/g CTAB surface area 80-139 m2/g BET/CTAB ratio 1.0-1.6 Sears No. (consumption of 5-25 ml 0.1 N NaOH) DBP No. 200-300 ml/100 g Al2O3 content <5% wk coefficient <3.4 Degraded particles <1.0 &mgr;m Non-degradable particles 1.0-100 &mgr;m is prepared by reacting alkali silicate with mineral acids and aluminum sulfate solution at temperatures of 60-95° C. at a pH of 7.0-10.0 while stirring constantly, wherein the reaction is continued to a solids concentration of 40-110 g/l, the pH is adjusted to a value between 3 and 5, and the precipitated silica is filtered off, washed and then dried, and optionally ground or granulated.
    Type: Grant
    Filed: September 3, 1999
    Date of Patent: July 31, 2001
    Assignee: Degussa AG
    Inventors: Anke Blume, Burkhard Freund, Bernhard Schwaiger, Mustafa Siray, Stefan Uhrlandt
  • Patent number: 6221149
    Abstract: The invention relates to a new process for the preparation of precipitated silica which has a very good dispersibility and very satisfactory reinforcing properties. It also relates to new precipitated silicas which are in the form of powder, of substantially spherical beads or of granules, these silicas being characterized by the fact that they have a CTAB specific surface of between 100 and 240 m2/g, a DOP oil uptake lower than 300 ml/100 g, a pore distribution such that the pore volume consisting of the pores whose diameter is between 175 and 275 Å represents less than 50% of the pore volume consisting of the pores of diameters which are smaller than or equal to 400 Å, a median diameter, after disintegration with ultrasound, smaller than 5 &mgr;m and an aluminum content of at least 0.35% by weight. The invention also relates to the use of the said silicas as reinforcing fillers for elastomers.
    Type: Grant
    Filed: August 24, 1998
    Date of Patent: April 24, 2001
    Assignee: Rhodia Chimie
    Inventors: Yves Bomal, Yvonick Chevallier, Philippe Cochet
  • Patent number: 6221326
    Abstract: A method for preparing hollow particles comprising a dense silica shell, by precipitating active silica from an aqueous alkaline metal silicate on a core constituted in a material other than silica and by eliminating the material without destroying the silica shell. The particles are used as insulating materials; as hollow fillers for polymers, building materials, rubber, paper, paint; as absorbing agents; as toothpaste abrasives or additives; as support for the absorption and/or graining out active matter, the liberation of the active matter being effected by the destruction of the silica core by mechanical rupture or by dissolving the silica shell in a basic medium or by diffusion; as sun screening agents or sun screening agent supports or for the formulation of liquid matter in solid form.
    Type: Grant
    Filed: October 20, 1998
    Date of Patent: April 24, 2001
    Assignee: Rhodia Chimie
    Inventor: Frédéric Amiche
  • Patent number: 6191122
    Abstract: A partially hydrophobic precipitated silica having a methanol wettability of 10 to 49%, in particular with a DBP uptake on a dry basis of greater than 250 g/100 g and a mean particle size of 1 to 12 &mgr;m and/or a carbon content of 0.3 to 1.85% and/or a loss on drying of 2.6 to 10.0% and/or a pH value of 5.5 to 10.0, is prepared by mixing the amount of water-repellent agent with the precipitated silica suspension at very short residence time and low pH value, filtering off the solid substance, washing free of salt, drying, post-treating thermally and milling. The partially hydrophobic precipitated silica can be used in active substance formulations and active substance formulations of hydrolysis-sensitive substance and in defoaming agents.
    Type: Grant
    Filed: March 28, 1997
    Date of Patent: February 20, 2001
    Assignee: Degussa Hüls Aktiengesellschaft
    Inventors: Heinz-Günter Lux, Karl Meier, Astrid Müller, Rolf Oelmüller, Anja Ramb
  • Patent number: 6187292
    Abstract: The invention discloses an abrasive precipitation silica useable in toothpaste compositions, said silica having a BET specific surface ranging from 15 to 300 m2/g, a DOP oil absorption ranging from 40 to 160 ml/g, a median particle diameter of at least 10 &mgr;m, generally ranging from 12 to 30 &mgr;m, a particle cohesion factor of at least 85% about for a median particle diameter ranging from 12 to 20 &mgr;m.
    Type: Grant
    Filed: February 19, 1999
    Date of Patent: February 13, 2001
    Assignee: Rhodia Chimie
    Inventors: Frédéric Amiche, Adrien Dromard
  • Patent number: 6171699
    Abstract: Essentially spherical silica-based granular particulates, whether having a mean particle size of at least 300 &mgr;m and a density of from 0.15 to 0.32, or a mean particle size of from 80 &mgr;m to 400 &mgr;m and a density of at least 0.32, are well adapted as reinforcing filler material for a variety of elastomeric matrices, e.g., rubber.
    Type: Grant
    Filed: March 7, 1995
    Date of Patent: January 9, 2001
    Assignee: Rhone-Poulenc Chimie
    Inventors: Michel Deleuil, Francois Parmentier
  • Patent number: 6171384
    Abstract: An amorphous silicate pigment having a pore volume of at least about 4.0 ml/g as measured by mercury intrusion, a BET surface area of at least about 300 m2/g, and an Al2O3 content of about 2.0-10.0 wt % is provided. The invention can be successfully used in recording media coatings, particularly coatings for recording media used in ink jet printing systems.
    Type: Grant
    Filed: May 4, 1998
    Date of Patent: January 9, 2001
    Assignee: J. M. Huber Corp.
    Inventors: Donald P. Conley, Gary W. Loock, Barry W. Preston, Michael C. Withiam
  • Patent number: 6146454
    Abstract: The invention relates to a new process for the preparation of precipitated silica which has a good dispersibility and very satisfactory reinforcing properties. It also relates to new precipitated silicas which are in the form of powder, of substantially spherical beads or of granules, these silicas being characterized by the fact that they have a CTAB specific surface of between 90 and 250 m.sup.2 /g, a BET specific surface of between 90 and 250 m.sup.2 /g, a DOP oil uptake lower than 300 ml/100 g, a zinc content of between 1 and 5% by weight, and by the fact that the number N of stearic acid molecules consumed per nm.sup.2 of silica surface, when stearic acid is reacted with this silica in xylene for 2 hours at 120.degree. C., is at least 1. The invention also relates to the use of the said silicas as reinforcing fillers for elastomers, especially for improving their rheological properties.
    Type: Grant
    Filed: February 11, 1999
    Date of Patent: November 14, 2000
    Assignee: Rhodia Chimie
    Inventors: Yves Bomal, Yvonick Chevallier, Evelyne Prat
  • Patent number: 6143066
    Abstract: The invention relates to a new process for the preparation of precipitated silica which has a good dispersibility and very satisfactory reinforcing properties. It also relates to new precipitated silicas which are in the form of powder, of substantially spherical beads or of granules, these silicas being characterized by the fact that they have a CTAB specific surface of between 90 and 250 m.sup.2 /g, a DOP oil uptake lower than 300 ml/100 g, a pore distribution such that the pore volume consisting of the pores whose diameter is between 175 and 275 .ANG. represents less than 50% of the pore volume consisting of the pores of diameters smaller than or equal to 400 .ANG., a zinc content of between 1 and 5% by weight and by the fact that the number N of molecules of stearic acid consumed per nm.sup.2 of silica surface, when stearic acid is reacted with the said silica in xylene for 2 hours at 120.degree. C., is at least 1.
    Type: Grant
    Filed: September 2, 1998
    Date of Patent: November 7, 2000
    Assignee: Rhodia Chimie
    Inventors: Yves Bomal, Yvonick Chevallier, Evelyne Prat
  • Patent number: 6120744
    Abstract: A process for preparing compounds of the formulae I and II ##STR1## where R.sup.1 and R have the meanings indicated in the specification by an addition reaction of a compound of the formula IIIR.sup.1 OH IIIwith an acetylene or allene of the formula IV or V ##STR2## in the gas phase at elevated temperatures in the presence of a heterogeneous catalyst. The catalyst is obtained by impregnating silica with a zinc salt, by a process in which the reaction is carried out at below 200.degree. C. and the catalyst contains, as an active component, an X-ray amorphous zinc silicate or cadmium silicate containing from 1 to 40% by weight, calculated as oxide, of zinc or cadmium, obtainable by applying a salt of zinc or cadmium and an inorganic oxo acid, which salt is decomposable at below 400.degree. C., to amorphous silica and forming the catalyst before the reaction at from 50 to 500.degree. C. or during the reaction in situ at from 50 to 200.degree. C.
    Type: Grant
    Filed: June 16, 1998
    Date of Patent: September 19, 2000
    Assignee: BASF Aktiengesellschaft
    Inventors: Joaquim Henrique Teles, Norbert Rieber, Klaus Breuer, Dirk Demuth, Hartmut Hibst
  • Patent number: 6107226
    Abstract: Essentially spherical precipitated silica beads, well adapted for the reinforcement of elastomeric matrices, have a mean particle size of at least 80 .mu.m, a BET specific surface area ranging from 60 to 130 m.sup.2 /g, a fill density in packed state ranging from 0.28 to 0.37, and a total pore volume ranging from 1.6 to 3.3 cm.sup.3 /g.
    Type: Grant
    Filed: May 2, 1990
    Date of Patent: August 22, 2000
    Assignee: Rhone-Poulenc Chimie
    Inventor: Yvonick Chevallier
  • Patent number: 6103942
    Abstract: A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours.
    Type: Grant
    Filed: April 8, 1999
    Date of Patent: August 15, 2000
    Assignee: Midwest Research Institute
    Inventors: Y. Simon Tsuo, Eugene P. Belov, Vadim G. Gerlivanov, Vitali V. Zadde, Solomonida I. Kleschevnikova, Nikolai N. Korneev, Eugene N. Lebedev, Akhsarbek B. Pinov, Eugene A. Ryabenko, Dmitry S. Strebkov, Eugene A. Chernyshev
  • Patent number: 6103209
    Abstract: Process for preparing porous spherical silica particles substantially consisting in emulsifying an acidic silica sol in a dispersing media, gelifying the microdrops of the sol in the emulsified state and submitting the resulting gel to thermal treatment in the presence of the emulsifier liquid and of sol gelation base.
    Type: Grant
    Filed: April 8, 1996
    Date of Patent: August 15, 2000
    Assignees: Enichem S.p.A., Eniricerche S.p.A.
    Inventors: Luigi Balducci, Raffaele Ungarelli
  • Patent number: 6071997
    Abstract: A three-dimensional composite of silica spheres interconnected by resin is provided having a three-dimensional network structure including silica particles having the following structural and dynamic characteristics and a resin present in the internal pores of said network:(a) three-dimensionally interconnected spherical silica particles having a diameter of 6 to 30 .mu.m;(b) on the surface of said spherical silica particles, a specific surface area of 300 to 400 m.sup.
    Type: Grant
    Filed: May 14, 1997
    Date of Patent: June 6, 2000
    Assignee: Agency of Industrial Science and Technology
    Inventors: Yuko Tanaka, Muneaki Yamaguchi, Hiromasa Ogawa, Katsutoshi Tanaka
  • Patent number: 6068825
    Abstract: Disclosed is an improvement in the process for the preparation of amorphous silicic acid particles useful, for example, as a filtration aid comprising the steps of a hydrothermal reaction to prepare calcium silicate particles and decalcification of the calcium silicate particles, after or without undertaking carbonation by the reaction of carbon dioxide, with an acid to form particles of amorphous silicic acid followed by drying of the amorphous silicic acid particles.
    Type: Grant
    Filed: December 17, 1998
    Date of Patent: May 30, 2000
    Assignee: Japan as represented by Director General of Agency of Industrial Science and Technology
    Inventor: Shuji Tsunematsu
  • Patent number: 6013234
    Abstract: Dry, freely-flowing, water-insoluble but readily dispersible, solid and homogeneous silica pigment particulates essentially spheroidal in geometrical configuration and having a mean particle size in excess of 80.mu., preferably in excess of 150.mu., are prepared by atomizing to dryness a pulverulent aqueous suspension of silica having a solids contact in excess of 18%. Such silica pigment particulates, advantageously comprised of precipitated silica, are well adapted as reinforcing fillers for elastomeric matrices.
    Type: Grant
    Filed: June 7, 1995
    Date of Patent: January 11, 2000
    Assignee: Rhodia Chimie
    Inventors: Jean-Louis Ray, Maurice Coudurier
  • Patent number: 6001322
    Abstract: Precipitated silica particulates suited for homogeneous incorporation, dispersion and distribution within vulcanized elastomeric matrices reinforced therewith can be formed as either a powder, substantially spherical beads, or granulates. The silica particulates have a CTAB specific surface ranging from 100 to 140 m.sup.2 /g, a median diameter .phi..sub.50, after ultrasonic disintegration, less than 2.8 .mu.m, an ultrasonic disintegration factor F.sub.D greater than 3 ml, a BET specific surface ranging from 100 to 200 m.sup.2 /g, a mean particle size greater than 15 .mu.m when formed as a powder, at least 80 .mu.m when formed a s substantially spherical beads, and at least 1 mm when formed as a granulate, a packing density in the tamped state of at least 0.17, and a DOP oil uptake ranging from 150 to 400 ml/100 g.
    Type: Grant
    Filed: September 21, 1998
    Date of Patent: December 14, 1999
    Assignee: Rhone-Poulenc Chimie
    Inventors: Yvonick Chevallier, Evelyne Prat
  • Patent number: 5989510
    Abstract: A method of directly precipitating a spherical amorphous silica in a high yield by adding a carboxymethyl cellulose (CMC) as a coagulation growing agent in a step of neutralizing the alkali silicate with an acid. The CMC having a particular etherification degree and a particular polymerization degree is added in an amount of from 1 to 100% by weight reckoned as SiO.sub.2 with respect to silica in the alkali silicate, whereby the whole silica particles turn into spherical amorphous silica particles having high sphericalness. There can be obtained spherical amorphous silica particles having a BET specific surface area of from 25 to 800 m.sup.2 /g, an apparent specific gravity of from 0.1 to 0.8 and a particle diameter of from 0.2 to 50 .mu.m cheaply and in a high yield.
    Type: Grant
    Filed: June 17, 1996
    Date of Patent: November 23, 1999
    Assignee: Mizusawa Industrial Chemical, Ltd.
    Inventors: Kiyoshi Abe, Kazuhiko Suzuki, Hiroshi Ogawa
  • Patent number: 5989524
    Abstract: Silica compatible with flavors, exhibiting, at an RP/DA abrasivity lower than or equal to 10, a compatibility with flavors which is higher than 10% and, at an RP/DA abrasivity higher than 10, a compatibility with flavors of at least 30%. Process for the preparation of flavor-compatible silica by treating the surface of a silica originating from the reaction of an alkali metal silicate with an inorganic or organic acidic agent, the silica being in dry form or in an aqueous suspension, with the aid of an organic compound capable of developing hydrogen bonds or ionic bonds with, respectively, the Si--OH silanol groups or the SiO.sup.- anionic groups at the surface of the said silica to be treated, the said treated silica being subsequently, if necessary, isolated and/or washed and/or dried. Use in dentifrice compositions and dentifrice compositions including the said silica.
    Type: Grant
    Filed: July 18, 1997
    Date of Patent: November 23, 1999
    Assignee: Rhodia Chimie
    Inventors: Adrien Dromard, Jean-Francois Viot
  • Patent number: 5968470
    Abstract: Precipitated silica particulates having a BET specific surface ranging from 20 to 300 m.sup.2 /g, a CTAB specific surface ranging from 10 to 200 m.sup.2 /g, an oil uptake (DBP) ranging from 80 to 400 cm.sup.3 /100 g, a pore volume ranging from 1 to 10 cm.sup.3 /g and a mean pore diameter ranging from 10 to 50 nm, well adapted for such applications as the coating of paper and catalysis, are prepared by (a) simultaneously introducing a silicate and an acid into a dispersion of colloidal silica, thereby providing a silica suspension, (b) next decreasing the pH of such suspension to a value ranging from 3 to 7, and (c) then separating the silica particulates from the final suspension and drying them.
    Type: Grant
    Filed: April 13, 1994
    Date of Patent: October 19, 1999
    Assignee: Rhone-Poulenc Chimie
    Inventor: Jacques Persello
  • Patent number: 5968249
    Abstract: A process for preparation of silica pigment by mixing sea water and an aqueous solution of sodium silicate is disclosed, in which no acidulating agent is used and the amount of sea water is 50-500 times of the sodium silicate by weight.
    Type: Grant
    Filed: January 16, 1998
    Date of Patent: October 19, 1999
    Inventor: Ju Chen Liang
  • Patent number: 5964937
    Abstract: An amorphous silica having an RDA value of between 30 and 70, an oil absorption capacity of between 100 and 155 cc/100 g and a moisture loss of less than 7% w/w, can be incorporated at a 10% to 25% loading into a transparent toothpaste having a refractive index of above 1.445, this toothpaste having an RDA value of between 30 and 60.
    Type: Grant
    Filed: December 23, 1997
    Date of Patent: October 12, 1999
    Assignee: Crosfield Limited
    Inventor: Peter William Stanier
  • Patent number: 5958127
    Abstract: The invention relates to a new process for the preparation of precipitated silica which has a good dispersibility and very satisfactory reinforcing properties. It also relates to new precipitated silicas which are in the form of powder, of substantially spherical beads or of granules, these silicas being characterized by the fact that they have a CTAB specific surface of between 90 and 250 m.sup.2 /g, a BET specific surface of between 90 and 250 m.sup.2 /g, a DOP oil uptake lower than 300 ml/100 g, a zinc content of between 1 and 5% by weight, and by the fact that the number N of stearic acid molecules consumed per nm.sup.2 of silica surface, when stearic acid is reacted with this silica in xylene for 2 hours at 120.degree. C., is at least 1. The invention also relates to the use of the said silicas as reinforcing fillers for elastomers, especially for improving their rheological properties.
    Type: Grant
    Filed: March 3, 1997
    Date of Patent: September 28, 1999
    Assignee: Rhone-Poulenc Chimie
    Inventors: Yves Bomal, Yvonick Chevallier, Evelyne Prat
  • Patent number: 5958577
    Abstract: The method for producing a bulk silica porous material is presented. The obtained material has a large crystal size serving to reduce light scattering, and uniform and adjustable pore size. This can be utilized for optical and electronic functional materials. The method comprises the steps of:forming a silica/surfactant composite by mixing starting materials containing an alkoxysilane, water and a surfactant and allowing to the starting materials to react;maturing said silica/surfactant composite by allowing the same to stand in a closed container to effect the development of a silica network structure and the formation of porous structure in said composite;drying said matured silica/surfactant composite for removing the solvent and for condensation of said matured silica/surfactant composite; and,sintering said condensed silica/surfactant composite to remove the surfactant to obtain a silica porous material.
    Type: Grant
    Filed: January 6, 1998
    Date of Patent: September 28, 1999
    Assignee: Kabushiki Kaisha Toyota Chuo Kenkyusho
    Inventors: Noriaki Sugimoto, Shinji Inagaki, Yoshiaki Fukushima, Tatsumi Hioki, Makoto Ogawa
  • Patent number: 5939051
    Abstract: Oral compositions, such as oral gels and toothpastes, containing a novel high cleaning, low abrasion silica hydrogel abrasive.
    Type: Grant
    Filed: February 27, 1998
    Date of Patent: August 17, 1999
    Assignee: Colgate-Palmolive Company
    Inventors: John Santalucia, Peter Ren, Nagaraj Dixit, Gary Durga, Michael Prencipe, Mahmoud Hassan, Marcus Bentley, Barry Self
  • Patent number: 5935543
    Abstract: Amorphous precipitated silica which may be used to form battery separators of very low specific resistance is characterized by (a) a CTAB surface area in the range of from 140 to 185 m.sup.2 /g; (b) a DBP oil absorption in the range of from 210 to 310 cm.sup.3 /100 g; (c) a mean ultimate particle size in the range of from 10 to 18 nm; (d) a total intruded volume in the range of from 2.6 to 4 cm.sup.3 /g; and (e) an intruded volume in the range of from 0.9 to 2 cm.sup.3 /g for pores having diameters in the range of from 20 to 100 nm.
    Type: Grant
    Filed: August 8, 1997
    Date of Patent: August 10, 1999
    Assignee: PPG Industries Ohio, Inc.
    Inventors: James L. Boyer, Thomas G. Krivak, Robert C. Wang, Laurence E. Jones
  • Patent number: 5932191
    Abstract: The present invention relates to silicas, in particular precipitated silicas, which can be used in particular as abrasive agents in toothpaste compositions. The silicas according to the invention have, first of all, low specific surfaces. Their BET specific surface is between 20 and 75 m.sup.2 /g, preferably between 35 and 64 m.sup.2 /g. The invention also relates to a process for their preparation and to the toothpaste compositions containing them.
    Type: Grant
    Filed: July 31, 1996
    Date of Patent: August 3, 1999
    Assignee: Rhone-Poulenc Chimie
    Inventors: Yvonick Chevallier, Adrien Dromard
  • Patent number: 5922298
    Abstract: Amorphous precipitated silica which may be used to form battery separators of very low shrinkage is characterized by (a) a BET surface area in the range of from 60 to 200 m.sup.2 /g; (b) a CTAB surface area in the range of from 40 to 150 m.sup.2 /g; (c) a DBP oil absorption in the range of from 180 to 300 cm.sup.3 /100 g; (d) a mean ultimate particle size in the range of from 20 to 30 nm; (e) a total intruded volume in the range of from 2.5 to 4 cm.sup.3 /g; (f) an intruded volume in the range of from 0.3 to 1.2 cm.sup.3 /g for pores having diameters in the range of from 20 to 100 nm; and (g) a pore diameter at the maximum of the volume pore size distribution function in the range of from 30 to 200 nm.
    Type: Grant
    Filed: August 8, 1997
    Date of Patent: July 13, 1999
    Assignee: PPG Industries Ohio, Inc.
    Inventors: James L. Boyer, Thomas G. Krivak