WO2013043570A1 - Particule de silice contenant du soufre - Google Patents

Particule de silice contenant du soufre Download PDF

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Publication number
WO2013043570A1
WO2013043570A1 PCT/US2012/055865 US2012055865W WO2013043570A1 WO 2013043570 A1 WO2013043570 A1 WO 2013043570A1 US 2012055865 W US2012055865 W US 2012055865W WO 2013043570 A1 WO2013043570 A1 WO 2013043570A1
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Prior art keywords
composition
compound
molar ratio
following
sulfur
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PCT/US2012/055865
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English (en)
Inventor
Nicholas S ERGANG
Bruce A Keiser
Richard Mimna
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Nalco Company
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Priority claimed from US13/242,599 external-priority patent/US8333835B2/en
Application filed by Nalco Company filed Critical Nalco Company
Publication of WO2013043570A1 publication Critical patent/WO2013043570A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume

Definitions

  • This invention disclosure pertains generally to a silica-containing composition, and more specifically to a silica-containing composition that includes a sulfur moiety.
  • the invention has particular relevance to silica-containing compositions that further include a metal or metalloid cation and an optional organosilane moiety.
  • Silica-containing materials have ubiquitous applications. More specifically, a variety of manufacturing processes that produce either consumer or industrial products utilize silica- containing materials for various purposes. For example, silica-containing products can be utilized as fillers in coatings (e.g. paints) and polymer composites, catalysts supports, beer/wine/juice clarifiers. New and improved silica-containing products with increased performance and ease of use are desired by various industries. SUMMARY OF THE INVENTION
  • the present invention accordingly provides for a composition
  • a composition comprising a compound having the following formula (Si02) x (OH) y M z S a F: wherein M is at least one of the following metal or metalloid cations: boron, magnesium, aluminum, calcium, titanium, vanadium.
  • S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarbamates, polymer-based dithiocarbamates, and polysulfide salts; wherein F optionally exists and said F is at least one of the following: a functionalized organosilane, a sulfur-containing organosilane, an amine-containing organosilane, and an alkyl-containing organosllane at a surface area coverage of about 0.01 to aboutlOQ %; and wherein the molar ratio of /x is equal to about 0.01 to about 0,5, the molar ratio of x/z is equal to about 0.5 to about 300 or from about 0,5 to about 100, and the molar ratio of a ' z is about 0,5 to about 5,
  • the present invention also provides tor a composition comprising a compound having a formula of: (Si0 )i 5 -Cui S 5 .
  • the present invention further provides for a product produced by filtering an aqueous- based material from a composition
  • a composition comprising a compound having the following formula (Si02) x (OH)yM z S a F wherein M is selected from at least one of the following metal or metalloid cations; boron, magnesium, aluminum, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold, and bismuth; wherein S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarbamates, polymer-based dithiocarbamat.es, and polysulfide salts; wherein F optionally exists and said F is at least one of the following: a functional ized organosilane, a sulfur-containing organosilane, an amine-containing organosilane, and an
  • the present invention also provides for a product produced from drying a composition at a temperature of about 100 °C to about 350 °C, wherein said composition comprises a compound containing the following formula (Si02) x (OH)yM z S s F: wherein M is selected from at least one of the following metal or metalloid cations: boron, magnesium, aluminum, calcium, titanium, vanadium, manganese, iron, cobalt nickel, copper, zinc, zirconium, molybdenum., palladium, silver, cadmium, tin, platinum, gold, and bismuth; wherein S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarbamates, polymer-based dithiocarbamates, and polysulfide salts; wherein F optionally exists and said F is at least one of the following; a functionalized organosilane, a sulfur-containing organosilane, an amine- containing organosilane
  • the present invention provides for a method of forming a silica-containing product/ composition
  • a. providing a silica-containing precursor (SCP) contained in solution that has a pH less than or equal to a pH of about 7; b. optionally doping the SCP with one or more metal species, wherein said doping occurs when the solution has a pH less than or equal to a pH of about 7; e, adj u sting the pH of the solution to greater than about 7; d, adding an effective amount of salt to the solution so that the conductivity of the solution is greater than or equal to about 4 raS, wherein said addition occurs prior to, simultaneous with, or after the pH adjustment in step lc; e.
  • SCP silica-containing precursor
  • step e optionally filtering and drying the SCP; and f. optionally reacting the dried product from step e with a functional group and optionally wherein the resultant functionalized dried product is at least one of the following: a functionalized metal oxide-doped or metal sulfide- doped silica-containing product.
  • the present invention also provides for a method of forming a silica-containing product/composition comprising: a. providing a silica-containing precursor (SCP) contained in solution that has a pH greater than 7; b. adjusting the pH of the solution to less than or equal to about 7; c. optionally doping the SCP with one or more metal species, wherein said doping occurs when the solution has a pH less than or equal to a pH of about 7; d. adjusting the pH of the solution to greater than about 7; e, adding an effective amount of salt to the solution so that the conductivity of the solution is greater than or equal to about 4 mS, wherein said addition occurs prior to, simultaneous with, or after the pH adjustment in step 2d; f.
  • SCP silica-containing precursor
  • step f optionally filtering and drying the SCP; and g. optionally reacting the dried product from step f with a functional group and optionally wherein the resultant functionalized dried product is at least one of the following: a functionalized metal oxide-doped or metal sulfide-doped silica-containing product.
  • the present invention provides a composition that contains a compound with a sulfur component, specifically a compound having a formula of (Si0 2 ) x (OH) y M z S a .F: wherein M is selected from at least one of the following metal or metalloid cations: boron, magnesium, aluminum, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold, and bismuth; wherein S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarbamates, and polymer-based dithioearbamates, polysulfide salts; wherein F optionally exists and said F is at ieast one of the following: a functionalized organosilane, a sulfur-containing organosilane, an amine-containing organosilane, and an alkyl-containing organsilane
  • the compound can be in various forms and proportions relative to the components of the compositions, in addition, various products can contain the compounds encompassed by this invention.
  • the following compound embodiments can stand alone, be further modified by chemical and/or physical means, or integrated into other products (e.g., consumer or industrial products).
  • the invention also provides for a composition
  • a composition comprising a compound having a formula of: (Si0 2 )i5(OH) y 'Cu;S 5i where y is the surface concentration of hydroxy! species as determined by moisture content.
  • the compound comprises about 3 % to about 15 % by weight in an aqueous-based slurry.
  • the compound comprises about 15% to about 40% by weight in a wet cake form.
  • the compound in another embodiment, comprises about 40% to about 99% by weight in a powder form, In embodiments, the compound comprises about 60% to about 99% by weight in a powder form.
  • the compound has a particle size of about 5 to about 200 ⁇ containing aggregated nanoparticles ranging from about 3 to about 500nm. In embodiments, the compound has a particle size of about 5 to about 500 am containing aggregated nanoparticles ranging from about 3 to about 500 nm.
  • the compound has a surface area of about 30 m'/g to about 800 m 2 /g. In embodiments, the compound has a surface area of about 2 m 2 /g to about 200 m7g or from about 2 m 2 /g to about 400 m 2 /g.
  • the compound in another embodiment, has a pore volume of about 0.3 cc/g to about 2.0 cc/g. In embodiments, the compound has a pore volume of about 0.01 cc/g to about 1.0 cc/g in another embodiment, a product is produced by filtering an aqueous-based material from a composition comprising a compound having the following formula (Si0 2 ) x (OH).,M z S a F wherein M is selected from at least one of the following: boron, magnesium, aluminum, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold, and bismuth; wherein S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarbamates, polymer-based dithiocarbamates, and polysulfide salts; wherein F optionally exists and
  • the product is produced from drying a composition at a temperature of about 100 °C to about 350 °C, wherein said composition comprises a compound having the following formula (Si0 2 ) x (OH)yM z SaF: wherein M is at least one of the following metal or metalloid cations: boron, magnesium, aluminum, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin.
  • S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarhamates, polymer-based dithiocarbamates, and pol suifide salts; wherein F optionally exists and said F is at least one of the following: a functionalized organosilane, a sulfur-containing organosilane, an amine-containing organosilane, and an aikyl-containing organosilane at a surface area coverage of about 0,01 to about 100 %; and wherein the molar ratio of y/x is equal to about 0.01 to about 0.5, the molar ratio of x/z is equal to about 0.5 to about 300 or from about 0.5 to about 100, and the molar ratio of a/z is about 0,5 to about 5.
  • S is a sulfur-based species selected from at least one of the following: sulfide salts, dithiocarhamates, polymer-based dithiocarbamates, and pol suifide salts
  • the compounds can be made in various ways, such as U.S. Patent Application Publication No. 2007/0231249, which is herein incorporated by reference.
  • silica-containing products encompassed by this invention can be made by the following methods.
  • One methodology involves starting from an acidic starting point,
  • the method comprises forming a silica-containing product comprising the steps of: a, providing a silica-containing precursor (SCP) contained in solution that has a pH less than or equal to a pH of 7; b, optionally doping the SCP with one or more metal species, wherein said doping occurs when the solution has a pH less than or equal to a pH of 7; e, adjusting the pH of the solution to greater than 7; d, adding an effective amount of salt to the solution so that the conductivity of the solution is greater than or equal to 4 mS, wherein said addition occurs prior to, simultaneous with, or after the pH adjustment in step k; e. optionally filtering and drying the SCP; and f.
  • SCP silica-containing precursor
  • step f optionally reacting the dried product from step e with a functional group and optionally wherein the resultant functionalized dried product is at least one of the following: a functionalized metal oxide-doped or metal sulfide-doped silica-containing product.
  • the functional group in step f is an organosilane.
  • the silicon-containing precursor is selected from at. least one of the following; silicic acid, colloidal silica, tetraethylorthosilicate, and dispersed fumed silica, in another embodiment, the pH range of the SCP in step 1(a) is from 3 to 4.
  • the pH of the SCP is adjusted to greater than 7 by mixing/interacting the molecules of said SCP with an alkaline solution at a shear rate of 6 to 23 ffl/s based on tip speed.
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by mixing said SCP with an alkaline solution via a mixing chamber.
  • a mixing chamber is described in U.S. Patent No.
  • the mixing chamber comprises a first conduit having one or more inlets and outlets; a second conduit having one or more inlets and outlets, wherein said first conduit secures to said second conduit and traverses said second conduit; a mixing chamber that has one or more inlets and outlets, wherein said second conduit secures to said mixing chamber and wherein said outlets of said first conduit and said outlets of said second conduit are in communication with said mixing chamber: and an adaptor that is in communication with said outlet of said mixing chamber and is secured to said mixing chamber.
  • the mixing chamber can then be attached or in communication with a receptacle that holds/processes through (e.g. a conduit) a mixed product, in one embodiment, said mixing chamber can then be attached or in communication with a receptacle that holds/processes a mixed product resulting from said pH adjustment of said SCP.
  • Ultra Turax Model Number lJTI-25 (available from 1KA® Works, Inc. i Wilmington, NC), a mixing device, can be utilized.
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution with mixing yielding a Reynolds Number greater than or equal to 2,000 to form the siiica-coniaining product.
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution under transitional flow conditions (i.e., Reynolds Numbers between 2,000 and 4,000) to form the silica-containing product.
  • transitional flow conditions i.e., Reynolds Numbers between 2,000 and 4,000
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution under turbulent flow conditions (i.e., Reynolds Numbers greater than or equal to 4,000) to form the silica-containing product.
  • turbulent flow conditions i.e., Reynolds Numbers greater than or equal to 4,000
  • the pH of the SCP is adjusted to a pH range of about 7 to about. 1 1 with the use of a chemistry selected from at least one of the following: ammonium hydroxide, ammonium carbonate, mineral bases such as but. not limited to sodium hydroxide and/or potassium hydroxide, organic bases such as but not limited to irimethylammonium hydroxide, alkaline silicates, sulfide salts such as but not limited to sodium sulfide, and polysuifide containing salts such as but not limited to calcium polysuifide and/or sodium polysuifide.
  • a chemistry selected from at least one of the following: ammonium hydroxide, ammonium carbonate, mineral bases such as but. not limited to sodium hydroxide and/or potassium hydroxide, organic bases such as but not limited to irimethylammonium hydroxide, alkaline silicates, sulfide salts such as but not limited to sodium sulfide, and polysuifide
  • the resulting slurry from step d is filtered and dried such that the solid concentration of said dried and filtered product is increased from about 5 wt% to about 99 wt%.
  • the dried product from step e is surface treated with an organosilane via controlled hydrolysis and condensation of the silane to the silica surface in at least one of the processes: an organic solvent, supercritical solvent, or solvent-free process.
  • Another methodology involves starting from an alkaline starting point.
  • the method comprises forming a silica-containing product comprising the steps of: a, providing a silica-containing precursor (SCP) contained in solution that has a pH greater than about 7; b. adjusting the pH of the solution to less than or equal to about 7; c. optionally doping the SCP with one or more metal species, wherein said doping occurs when the solution has a pH less than or equal to a pH of about 7; d. adjusting the pH of the solution to greater than about 7; e. adding an effective amount of salt to the solution so that the conductivity of the solution is greater than or equal to about 4 mS, wherein said addition occurs prior to, simultaneous with, or after the pH adjustment in step 2d; f.
  • SCP silica-containing precursor
  • step f optionally filtering and drying the SCP; and g. optionally reacting the dried product from step f with a functional group and optionally wherein the resultant functionalized dried product is at least one of the following: functionalized metal oxide-doped or metal sulfice-doped silica-containing product.
  • the functional group in step g is an organosilane.
  • the silicon-containing precursor is selected from at least one of the -following: silicic acid, colloidal silica, alkaline silicates, tetraethylorthosilicate, and dispersed fumed silica.
  • the pH of the silicon-containing precursor is adjusted through the use of at least one of the following: carbonic acid, an organic acicl(s) such as but not limited to i acetic acid, a mineral acid(s) such as but not limited to sulfuric acid and/or hydrochloric acid such that the pH is decreased to a range of from to about 2 to about 7.
  • the pH range of the SCP is adjusted to a range of about 3 to about 4 with acetic acid.
  • the pH of the SCP is adjusted to a pH range of about 7 to about 1 1 with the use of a chemistry selected from at least one of the following: ammonium hydroxide, ammonium carbonate, mineral bases, organic bases, alkaline salts, sulfide salts, alkaline silicates, and poiysulfide containing salts.
  • a chemistry selected from at least one of the following: ammonium hydroxide, ammonium carbonate, mineral bases, organic bases, alkaline salts, sulfide salts, alkaline silicates, and poiysulfide containing salts.
  • the resulting shiny from step e is filtered and dried such that the solid concentration of said dried and filtered product is increased from about 5 wt% to about 99 wt%.
  • the dried product from step f is surface treated with an organosilane via controlled hydrolysis and condensation of the siiane to the surface of the SCP in at least one of the following: an organic solvent, supercritical solvent, or solvent-free process.
  • the pH of the SCP is adjusted to greater than about 7 by mixing said SCP with an alkaline solution at a shear rate of about 6 to about 23 m/s based on tip speed.
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by mixing said SCP with an alkaline solution via a mixing chamber.
  • a mixing chamber is described in U.S. Patent No. 7,550,060, "Method and Arrangement for Feeding Chemicals into a Process Stream".
  • the mixing chamber comprises a first conduit having one or more inlets and outlets; a second conduit having one or more inlets and outlets, wherein said first conduit secures to said second conduit and traverses said second conduit; a mixing chamber that has one or more inlets and outlets, wherein said second conduit secures to said mixing chamber and wherein said outlets of said first conduit and said outlets of said second conduit are in communication with said mixing chamber; and an adaptor that is in communication with said outlet of said mixing chamber and is secured to said mixing chamber.
  • the mixing chamber can then be attached or in communication with a receptacle that holds/processes through (e.g. a conduit) a mixed product.
  • said mixing chamber can then be attached or in communication with a receptacle that holds/processes a mixed product resulting from said pH adjustment of said SCP.
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution with mixing yielding a Reynolds Number greater than or equal to 2,000, to form the silica-containing product,
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution under transitional flow conditions (i.e., Reynolds Numbers between 2,000 and 4,000) to form the silica -contain g product.
  • transitional flow conditions i.e., Reynolds Numbers between 2,000 and 4,000
  • the method further comprises adjusting the pH of the SCP to greater than about 7 by combining said SCP with an alkaline solution under turbulent flow conditions (i.e., Reynolds Numbers greater than or equal to 4,000) to form the silica-containing product.
  • the sulfur-based species of the present invention may be selected from a representative list but not intended to be a limiting list of at least one of the following: sulfide salts, dithiocarbamates, polymer-based dithiocarbamates, and polysulfide salts.
  • Sulfide salts maybe but not limited to sodium sulfide, potassium sulfide, and/or metal sulfides such as copper sulfide
  • Dithiocarbamates may be but not limited to dimethyldithlocarbamate (DMDTC) or diethyldithiocarbamate (DEDTC).
  • Polymer-based dithiocarbamates contain organic polymers containing the functional group nCS?. wherein R is an alkyl group which is linear or branched.
  • R is an alkyl group which is linear or branched.
  • An example of a commercially available polymer-based dithiocarbamate is described in U.S. Patent Nos. 5,164,095 and U.S. Patent Nos. 5,346,627, which are herein incorporated by- reference.
  • Polysulfides that can be used in the present invention include, but are not limited to, sodium polysulfide and calcium polysulfide.
  • Organosilanes that can be used in the current invention are well known in the art and may be represented generally by R (4 , a rSiX a , wherein a may be from 1 to 3.
  • the organo-functional group, R- may be any aliphatic or alkene containing functionalized group such as propyl, butyl, 3-chloropropyi. amine, thiol, and combinations thereof.
  • X is representative of a hydrolysabie alkoxy group, typically methoxy or ethoxy. Some examples are 3-thiopropyl and mercaptopropyl silanes.
  • salt is added to increase the conductivity of the reaction solution to 4mS.
  • the salts include, but are not limited to, alkali and alkaline halides, sulfates, phosphates, and nitrates such as sodium sulfite, potassium chloride, sodium chloride, sodium nitrate, calcium sulfate, and potassium phosphate.
  • alkali and alkaline halides, sulfates, phosphates, and nitrates such as sodium sulfite, potassium chloride, sodium chloride, sodium nitrate, calcium sulfate, and potassium phosphate.
  • the effective amount of salt added to reach the desired conductivity will vary dependent on the salt of choice.
  • Thiols and amines are represented generally by the class of organi and inorganic compounds containing the amine or thiol group having the general formula -B-(SH) or -B- (NHb), wherein B is a linear or branched group consisting of carbon atoms such as -((3 ⁇ 4) ⁇ , wherein n is from 1 to 15. in particular where n is 1 to 6, and most preferred where n is 3.
  • a solution containing 16.4 g of a 25 wt% ammonia solution and 5,84 g ammonium carbonate was prepared in 24,6 g DI water.
  • the solution was added to the reaction flask quickly whereupon the viscosity of the solution increased significantly.
  • the mixture was stirred for 30 minutes, then any remaining silicic acid was fed at 20 ml/min, Upon completion of the silicic acid feed, the heating was turned off and the solution was allowed to cool.
  • the silica slurry was filtered and feeze-dried at 1 50 °C to produce a dry powder.
  • Nitrogen sorption analysis of the powder was performed on an Autosorb-lC unit from Quantachrome.
  • the sample was degassed at 300 °C for 2 h, then characterized by a multi-point BET (Brunauer, Emmett, and Teller - a surface area test) surface area, total pore volume, and BJH (Barrett- Joyner-Halenda) adsorption pore size distribution.
  • Physical data indicated a surface area of 354 square meters per gram, a pore volume of 1.19 cc/g, and a pore diameter of 13.5 nm.
  • a solution containing 17.3 g sodium sulfide and 11.8 g of a 25 wt% ammonia was prepared in 200 g DI water.
  • the solution was quickly added to the reaction flask after 3 h of silicic acid feed where the viscosity of the solution increased significantly.
  • the mixture was stirred for 30 minutes, then any remaining silicic acid was fed at 16 ml/min. Upon completion of the silicic acid feed, the heating was turned off and the solution was allowed to cool.
  • the CuS-doped silica slurry was filtered and dried at 105 °C to produce a dry powder, Nitrogen sorption analysis of the powder was performed on an Autosorb-lC unit from Quantachrome. The sample was degassed at 1.05 °C for 4 h, then characterized by a multi-point BET surface area, total pore volume, and BJH adsorption pore size distribution, Nitrogen sorption analysis indicated a surface area of 321 square meters per gram, a pore volume of 1 ,46 cc/g, and a pore diameter of 18.2 nm,
  • the CuS-doped silica slum' was filtered and flash-dried at 565 °F to produce a dry powder.
  • Nitrogen sorption analysis of the powder was performed on an Autosorb-3C unit from Quantachrome. The sample was degassed at 105 °C for 4 h, then characterized by a multi-point BET surface area, total pore volume, and BJII adsorption pore size distribution. Nitrogen sorption analysis indicated a surface area of 227 square meters per gram, a pore volume of 0.45 cc/g, and a pore diameter of 7,9 nm.
  • three solutions are prepared: A) 2 kg Nalco N8691 silica sol, B) 53,2 g ferric sulfate and 60 g glacial acetic acid dissolved in 887 g DI water, and C) 184 g calcium polysulfide solution and 150 g 25 wt% ammonia dissolved in 2667 g DI water.
  • Solution B is added to solution A, followed by subsequent addition of solution C at a high shear rate, The mixture is stirred for 1-2 minutes before filtration.
  • the iron suifide-doped silica slurry is then filtered and flash-dried at 565 °F to produce a dry powder,
  • composition of matter claims include various combinations of sorbent components and associated compositions, such molar ratios of constituent particles.
  • the claimed compositions include combinations of the dependent claims, in a further embodiment, a range or equivalent thereof of a particular component shall include the individual component(s) within the range or ranges within the range.
  • the method of use claims include various combinations of the sorbent components and associated compositions, such molar ratios of constituent particles,
  • the claimed methods of use include combinations of the dependent claims.
  • a range or equivalent thereof of a particular component shall include the individual components) within the range or ranges within the range.
  • the method of manufacture claims include various combinations of the sorbent components and associated compositions, such pH control, in a further embodiment, the claimed methods of use include combinations of the dependent claims, in a further embodiment, a range or equivalent thereof of a particular component shall include the individual component(s) within the range or ranges within the range.

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  • Inorganic Chemistry (AREA)
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Abstract

L'invention concerne une composition contenant de la silice. La composition comporte un composé ayant la formule suivante : (SiO2)x(OH)yMzSaFB, dans laquelle : M est au moins l'un des cations métalliques ou métalloïdes suivants : bore, magnésium, aluminium, calcium, titane, vanadium, manganèse, fer, cobalt, nickel, cuivre, zinc, zirconium, molybdène, palladium, argent, cadmium, étain, platine, or et bismuth ; S est une espèce à base de soufre choisie parmi au moins l'un des suivants : sels sulfure, dithiocarbamates, dithiocarbamates à base de polymère et sels polysulfure ; F existe éventuellement et ledit F est au moins l'un parmi les suivants : un organosilane fonctionnalisé, un organosilane contenant du soufre, un organosilane contenant une amine et un organosilane contenant un alkyle à une couverture d'aire de surface d'environ 0,01 à environ 100 % ; le rapport molaire de y/x est égal à environ 0,01 à environ 0,5, le rapport molaire de x/z est égal à environ 0,5 à environ 300 ou d'environ 0,5 à environ 100 et le rapport molaire de a/z est d'environ 0,5 à environ 5 ; B est un solide hygroscopique à un rapport molaire eau à solide de 0,1 à 6 et de préférence comporte au moins un oxyde d'alcalino-terreux ou un oxyde de lanthanide.
PCT/US2012/055865 2011-09-23 2012-09-18 Particule de silice contenant du soufre WO2013043570A1 (fr)

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US13/242,599 US8333835B2 (en) 2010-04-08 2011-09-23 Sulfur containing silica particle

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