Titanium oxide particles and manufacturing method therefor

Patent metadata

Field	Value
Publication number	US-2021017037-A1
Application number	US-201916980456-A
Country	US
Kind code	A1
Filing date	Mar 27, 2019
Priority date	Mar 28, 2018
Publication date	Jan 21, 2021
Grant date	—

Abstract

The present invention manufactures titanium oxide particles that have a small degree of aggregation (size of aggregate particle diameter relative to primary particle diameter) and are not readily sintered by heating. The present invention has: a step in which an alkali and a solution including a carboxylic acid and a titanium (oxy)chloride are mixed, and the titanium (oxy)chloride is hydrolyzed by neutralization; and a step in which, after the hydrolysis by neutralization, the solution is heated to a temperature of 80° C. or more and 110° C. or less, and the titanium (oxy)chloride remaining in the solution is hydrolyzed by heating. It is thus possible to obtain titanium oxide particles that have a small degree of aggregation and a range of 1-35 for the ratio (D90/BET diameter) between the 90% cumulative mass particle size distribution diameter (D90) (nm) as measured by a dynamic light-scattering particle diameter distribution measurement device and the BET diameter (nm) as calculated from the specific surface area of the titanium oxide particles.

First claim

1 . A method for manufacturing titanium oxide particles, comprising:
a step of hydrolyzing a titanium (oxy)chloride by neutralization by mixing a solution containing a carboxylic acid and the titanium (oxy)chloride with an alkali; and a step of thermally hydrolyzing the titanium (oxy)chloride remaining in the solution after hydrolyzing the titanium (oxy)chloride by neutralization by heating the solution after hydrolyzing the titanium (oxy)chloride by neutralization at a temperature of 80° C. or more to 110° C. or less.

2 . The method according to claim 1 , wherein the solution containing the carboxylic acid and the titanium (oxy)chloride in the step of hydrolyzing the titanium (oxy)chloride by neutralization is heated at a temperature of 40° C. or more and 80° C. or less before being mixed, during being mixed, or after being mixed with the alkali.

3 . The method according to claim 1 , wherein in the step of hydrolyzing the titanium (oxy)chloride by neutralization, 0.1 to 50 mol % of the titanium (oxy)chloride is hydrolyzed, and then in the step of thermally hydrolyzing the titanium (oxy)chloride, the remaining titanium (oxy)chloride is hydrolyzed.

4 . Titanium oxide particles, wherein a ratio (D90/BET diameter) of a 90% cumulative volume particle size distribution diameter (D90) (nm) of the titanium oxide particles measured by a dynamic light scattering particle size distribution analyzer to a BET diameter (nm) calculated from a specific surface area of the titanium oxide particles is in a range of 1 to 35.

5 . The titanium oxide particles according to claim 4 , wherein the 90% cumulative volume particle size distribution diameter (D90) is in a range of 10 to 180 nm.

6 . The titanium oxide particles according to claim 4 , wherein a content of carbon contained in the titanium oxide particles is in a range of 0.4 to 10 mass %.

7 . The titanium oxide particles according to claim 4 , wherein a rutile ratio after the titanium oxide particles are heated at 600° C. for 2 hours is 10% or less.

8 . The titanium oxide particles according to claim 4 , wherein a BET specific surface area of the titanium oxide particles is 100 to 400 m 2 /g.

9 . The method according to claim 2 , wherein in the step of hydrolyzing the titanium (oxy)chloride by neutralization, 0.1 to 50 mol % of the titanium (oxy)chloride is hydrolyzed, and then in the step of thermally hydrolyzing the titanium (oxy)chloride, the remaining titanium (oxy)chloride is hydrolyzed.

10 . The titanium oxide particles according to claim 5 , wherein a content of carbon contained in the titanium oxide particles is in a range of 0.4 to 10 mass %.

11 . The titanium oxide particles according to 5, wherein a rutile ratio after the titanium oxide particles are heated at 600° C. for 2 hours is 10% or less.

12 . The titanium oxide particles according to 6, wherein a rutile ratio after the titanium oxide particles are heated at 600° C. for 2 hours is 10% or less.

13 . The titanium oxide particles according to 5, wherein a BET specific surface area of the titanium oxide particles is 100 to 400 m 2 /g.

14 . The titanium oxide particles according to 6, wherein a BET specific surface area of the titanium oxide particles is 100 to 400 m 2 /g.

15 . The titanium oxide particles according to 7, wherein a BET specific surface area of the titanium oxide particles is 100 to 400 m 2 /g.

Assignees

• Ishihara Sangyo Kaisha

Inventors

• Tomonari Masanori
• Ida Kiyonobu
• Hosokawa Takuya

Classifications

• C01P2006/80

  Compositional purity · CPC title

• C01P2006/12

  Surface area · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01G23/0538

  in the presence of seeds · CPC title