US 11,932,543 B2Granted

Composite oxide powder and method for production thereof

AssigneeTokuyama Corporation

InventorsHiromasa Fujioka, Hiroaki Taira, Osamu Tanaka

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Abstract

Composite oxide fine particles are produced by sol-gel method under conditions in which coarse particles and aggregated particles are unlikely to be generated, and the composite oxide fine particles are further wet-filtered using a filter to remove the coarse particles and the aggregated particles. Then, a salt is added to a dispersion of the composite oxide fine particles to produce weak aggregates of the composite oxide fine particles in the dispersion. A solid content is separated from the dispersion of the composite oxide fine particles containing the aggregates, and then dried. The solid content is easily made finer because no firm aggregates are generated during the drying. That is, composite oxide fine particles containing no coarse particles and aggregated particles are obtained. Use of a known cracking means can further reduce the amount of coarse particles.

Claims4

Dependent claims

A method for producing a silica-based composite oxide powder comprising a composite oxide of silicon and at least one metal selected from the group consisting of titanium and zirconium, the silica-based composite oxide powder having a volume-based cumulative 50% diameter measured by a laser diffraction scattering method in a range of 0.05 μm to 2.0 μm, and a coefficient of variation of 40% or less, wherein in a 5 mass % dispersion of the silica-based composite oxide powder obtained by ultrasonic irradiation (at an output of 40 W for 10 minutes), a content of particles having a particle diameter of 5 μm or more in a particle size distribution obtained by a Coulter counter method is 10 ppm or less on a number basis, the method comprising:

(1) preparing a partial hydrolysate of silicon alkoxide;
(2) mixing the partial hydrolysate with alkoxide of metal selected from the group consisting of titanium and zirconium or a mixture of the alkoxide of the metal and a complexing agent such that titanium or zirconium is mixed in a proportion of 50 mol % or less to a total amount of metal, thereby preparing a composite alkoxide material;
(3) hydrolyzing and condensing the composite alkoxide material in a dispersion medium containing water, thereby obtaining composite oxide particles;
(4) wet-filtering a dispersion of the composite oxide particles dispersed in the dispersion medium containing water using a filter medium having a pore size of 3 μm or more and 5 μm or less;
(5) adding a compound including at least one selected from the group consisting of carbon dioxide, ammonium carbonate, ammonium bicarbonate, and ammonium carbamate to the wet-filtered dispersion of the composite oxide particles to coagulate the composite oxide particles, thereby obtaining a coagulated composite oxide dispersion containing the coagulated composite oxide;
(6) separating the composite oxide particles from the coagulated composite oxide dispersion;
and
(7) drying the separated composite oxide particles.

5 more elements

A method for producing a silica-based composite oxide powder comprising a composite oxide of silicon and at least one metal selected from the group consisting of titanium and zirconium, the silica-based composite oxide powder having a volume-based cumulative 50% diameter measured by a laser diffraction scattering method in a range of 0.05 μm to 2.0 μm, and a coefficient of variation of 40% or less, wherein in a 5 mass % dispersion of the silica-based composite oxide powder obtained by ultrasonic irradiation (at an output of 40 W for 10 minutes), a content of particles having a particle diameter of 3 μm or more in a particle size distribution obtained by a Coulter counter method is 10 ppm or less on a number basis, the method comprising:

(1) preparing a partial hydrolysate of silicon alkoxide;
(2) mixing the partial hydrolysate with alkoxide of metal selected from the group consisting of titanium and zirconium or a mixture of the alkoxide of the metal and a complexing agent such that titanium or zirconium is mixed in a proportion of 50 mol % or less to a total amount of metal, thereby preparing a composite alkoxide material;
(3) hydrolyzing and condensing the composite alkoxide material in a dispersion medium containing water, thereby obtaining composite oxide particles;
(4) wet-filtering a dispersion of the composite oxide particles dispersed in the dispersion medium containing water using a filter medium having a pore size of 3 μm or more and 5 μm or less;
(5) adding a compound including at least one selected from the group consisting of carbon dioxide, ammonium carbonate, ammonium bicarbonate, and ammonium carbamate to the wet-filtered dispersion of the composite oxide particles to coagulate the composite oxide particles, thereby obtaining a coagulated composite oxide dispersion containing the coagulated composite oxide;
(6) separating the composite oxide particles from the coagulated composite oxide dispersion;
and
(7) drying the separated composite oxide particles.

5 more elements

Dependencies are inferred from the claim text.

Facts

Application: 16/978,299Filed 13 Mar 2019
Priority: JP 2018-04743515 Mar 2018
Published: US 2021/0009432 A114 Jan 2021
Granted: 19 Mar 2024
Term ends: Not estimatedThe source records don’t support an estimate.

Classification22 codes

C01B 33/145
Colloidal silica, e.g. dispersions, gels, sols: preparation of hydroorganosols, organosols or dispersions in an organic medium
C01B 33/20
Silicon; Compounds thereof: silicates
C01B 33/151
After-treatment of sols: by progressively adding a sol to a different sol, i.e. "build-up" of particles using a "heel"
C01B 33/18
Silica; Hydrates thereof, e.g. lepidoic silicic acid: preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof