Dispersion of particles of rutile titanium oxide, process for producing the same, and use of the same

Patent metadata

Field	Value
Publication number	US-9234113-B2
Application number	US-201013202404-A
Country	US
Kind code	B2
Filing date	Feb 15, 2010
Priority date	Feb 19, 2009
Publication date	Jan 12, 2016
Grant date	Jan 12, 2016

Abstract

The invention provides a dispersion of particles of rutile titanium oxide wherein the particles of rutile titanium oxide have a D50 in a range of 1 to 15 nm and a D90 of 40 nm or less in particle size distribution as determined by a dynamic light scattering method; a specific surface area in a range of 120 to 180 m 2 /g as determined by a BET method; and a rate of weight loss of 5% or less as obtained by heating the particles of rutile titanium oxide from 105° C. to 900° C.
Such a dispersion of particles of rutile titanium oxide is obtained by a process according to the invention, which comprises: a first step in which an aqueous titanium tetrachloride solution is heated and hydrolyzed to obtain a slurry containing the precipitated particles of rutile titanium oxide; a second step in which the slurry obtained in the first step is filtered and washed with water to remove water-soluble salts dissolved therein from the slurry; a third step in which the slurry obtained in the second step is subjected to a hydrothermal reaction in the presence of an organic acid; a fourth step in which the slurry obtained in the third step is filtered and washed with water; a fifth step in which an acid is added to the slurry obtained in the fourth step, and the resulting mixture is subjected to a wet dispersion treatment, thereby obtaining a dispersion; and a sixth step in which excess acid and water-soluble salts are removed from the dispersion obtained in the fifth step.

First claim

The invention claimed is:

1. A dispersion of particles of rutile titanium oxide in water wherein the particles of rutile titanium oxide have the following properties:
a D50 in a range of 1 to 15 nm and a D90 of 40 nm or less in particle size distribution as determined by a dynamic light scattering method;
a specific surface area in a range of 120 to 180 m 2 /g as determined by a BET method; and
a rate of weight loss of 5% or less as determined by heating the particles of rutile titanium oxide from 105° C. to 900° C.

2. A dispersion of particles of rutile titanium oxide in water as a dispersion medium wherein the particles of rutile titanium oxide have the following properties:
a D50 in a range of 1 to 15 nm and a D90 of 40 nm or less in particle size distribution as determined by a dynamic light scattering method;
a specific surface area in a range of 120 to 180 m 2 /g as determined by a BET method; and
a rate of weight loss of 5% or less as determined by heating the particles of rutile titanium oxide from 105° C. to 900° C.,
wherein the dispersion of particles of rutile titanium oxide is obtained by a process comprising:
a first step in which a chloride ion concentration of an aqueous titanium tetrachloride solution is adjusted to 4.4 mole/L or more and then is heated in a range between 86° C. to a boiling point to hydrolyze the titanium tetrachloride, wherein a slurry containing precipitated particles of rutile titanium oxide is obtained;
a second step in which the slurry obtained in the first step is filtered and washed with water, wherein dissolved water-soluble salts are removed from the slurry;
a third step in which the slurry from the second step is subjected to a hydrothermal reaction in the presence of an organic acid;
a fourth step in which the slurry from the third step is filtered and washed with water, wherein dissolved water-soluble salts are removed from the slurry;
a fifth step in which an acid is added to the slurry from the fourth step, and the resulting mixture is subjected to a wet dispersion treatment, wherein a dispersion is obtained; and
a sixth step in which excess acid and water-soluble salts are removed from the dispersion obtained in the fifth step, thereby providing a dispersion of particles of rutile titanium oxide in which the dispersion medium is water.

3. The dispersion of particles of rutile titanium oxide in water according to claim 2 , wherein the third step further comprises subjecting the slurry to a hydrothermal reaction in the presence of an organic acid in an amount of 75 parts by mole or more per 100 parts by mole of titanium oxide.

4. The dispersion of particles of rutile titanium oxide in water according to claim 2 , wherein the sixth step further comprises removing excess acid from the dispersion so that the dispersion has an electric conductivity in a range of 1 to 5 mS/cm.

5. The dispersion of particles of rutile titanium oxide in water according to claim 2 , wherein the hydrothermal reaction of the third step is carried out at a temperature in a range of 120-180° C.

6. The dispersion of particles of rutile titanium oxide in water according to claim 2 , wherein the first step comprises adjusting the chloride ion concentration of the aqueous solution of titanium tetrachloride to 7.0 mole/L or more.

7. A resin composition comprising the dispersion of particles of rutile titanium oxide according to claim 1 .

8. A process for producing a dispersion of particles of rutile titanium oxide according to claim 1 , which comprises:
a first step in which after a chloride ion concentration of an aqueous titanium tetrachloride solution is adjusted to 4.4 mole/L or more, the solution is heated at a temperature in a range of 86° C. to a boiling point to hydrolyze the titanium tetrachloride, thereby obtaining a slurry containing precipitated particles of rutile titanium oxide;
a second step in which the slurry obtained in the first step is filtered and washed with water to remove water-soluble salts dissolved therein from the slurry;
a third step in which the slurry obtained in the second step is subjected to a hydrothermal reaction in the presence of an organic acid;
a fourth step in which the slurry obtained in the third step is filtered and washed with water to remove water-soluble salts dissolved therein from the slurry;
a fifth step in which an acid is added to the slurry obtained in the fourth step, and the resulting mixture is subjected to a wet dispersion treatment, thereby obtaining a dispersion; and
a sixth step in which excess acid and water-soluble salts are removed from the dispersion obtained in the fifth step.

9. The process for producing a dispersion of particles of rutile titanium oxide according to claim 8 wherein the slurry is subjected to a hydrothermal reaction in the presence of an organic acid in an amount of 75 parts by mole or more per 100 parts by mole of titanium oxide in the third step.

10. The process for producing a dispersion of particles of rutile titanium oxide according to claim 8 wherein excess acid is removed from the dispersion so that the dispersion has an electric conductivity in a range of 1 to 5 mS/cm in the sixth step.

11. The process for producing a dispersion of particles of rutile titanium oxide according to claim 8 wherein the hydrothermal reaction is carried out at a temperature in a range of 120-180° C. in the third step.

12. The process for producing a dispersion of particles of rutile titanium oxide according to claim 8 wherein the chloride ion concentration of an aqueous solution of titanium tetrachloride is adjusted to 7.0 mole/L or more in the first step.

Assignees

• Nomura Atsushi
• Nakagawa Kenichi
• Morita Takanori
• Sakai Chemical Industry Co

Inventors

• Nomura Atsushi
• Nakagawa Kenichi
• Morita Takanori

Classifications

• Y10T428/2982

  Particulate matter [e.g., sphere, flake, etc.] · CPC title

• C01P2006/37

  Stability against thermal decomposition · CPC title

• C01P2006/12

  Surface area · CPC title

• C01G23/053 Primary

  Producing by wet processes, e.g. hydrolysing titanium salts · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title