Composite oxide powder and method for production thereof

Patent metadata

Field	Value
Publication number	US-11932543-B2
Application number	US-201916978299-A
Country	US
Kind code	B2
Filing date	Mar 13, 2019
Priority date	Mar 15, 2018
Publication date	Mar 19, 2024
Grant date	Mar 19, 2024

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.

First claim

The invention claimed is:

1. 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.

2. The method of claim 1 , further comprising:
(8) calcining the composite oxide particles obtained after the drying at 600° C. to 1200° C.

3. 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.

4. The method of claim 3 , further comprising:
(8) calcining the composite oxide particles obtained after the drying at 600° C. to 1200° C.

Assignees

• Tokuyama Corp

Inventors

• Fujioka Hiromasa
• Taira Hiroaki
• Tanaka Osamu

Classifications

• C01B33/20 Primary

  Silicates (persilicates C01B15/14 {; containing aluminium C01B33/26}) · CPC title

• C08K3/34

  Silicon-containing compounds · CPC title

• C08K9/06

  with silicon-containing compounds · CPC title

• C09C1/3081

  Treatment with organo-silicon compounds · CPC title

• C09C1/36

  Compounds of titanium {(C09C1/0009, C09C1/0015, C09C1/0078 take precedence)} · CPC title