Titanium oxide sol and process for producing same, ultrafine particulate titanium oxide, process for producing same, and uses of same
View Patent ↗A liquid phase method for producing titanium oxide sol by hydrolysis of titanium tetrachloride, which includes mixing an aqueous titanium tetrachloride solution into water at a temperature of 80° C. or higher within 60 seconds while maintaining the mixed solution at the temperature and cooling it to less than 60° C. within 15 minutes after the mixing is completed. Also disclosed is a titanium oxide sol obtained by the method, having an average primal particle diameter (D BET ) of 3 to 8 nm, a cumulative 50% volume particle diameter (D50 DLS ) and D BET have the relationship represented by D50 DLS =k×D BET where k is 1 or more and less than 5, and an anatase content of 70% or more; a particulate titanium oxide obtained by drying the titanium oxide sol; and a production method and application thereof to solar cells, lithium ion battery electrodes and dielectric materials.
1. A method for producing titanium oxide sol, comprising a process of mixing to completion an aqueous titanium tetrachloride solution into water at a temperature of 80° C. or higher within 100 seconds while maintaining the mixed solution at the temperature and cooling it to less than 60° C. within 15 minutes after the mixing is completed in a method for producing titanium oxide sol by the hydrolysis of titanium tetrachloride in the liquid phase method.
2. The method for producing titanium oxide sol as claimed in claim 1 , comprising a step of mixing an aqueous titanium tetrachloride solution into water at a temperature of 80° C. or higher within 60 seconds while maintaining the mixed solution at the temperature and cooling it to less than 60° C. within 15 minutes after the mixing is completed.
3. The method for producing titanium oxide sol as claimed in claim 1 , comprising a dechlorination step of separating titanium oxide and hydrochloric acid generated by the hydrolysis reaction using at least one of the ultrafiltration membrane, reverse osmosis membrane, ion-exchange resin and electrodialysis membrane.
4. Titanium oxide sol obtained by the method as claimed in claim 1 having an average primal particle diameter (D BET ) calculated from the BET specific surface area of 3.75 to 5 nm, wherein the cumulative 50% volume particle diameter (D50 DLS ) measured by the dynamic light scattering method and D BET have the relationship represented by the following formula (1):
D 50 DLS =k×D BET (1)
(in the formula, k is a value of 1 or more and less than 5).
5. The titanium oxide sol as claimed in claim 4 , wherein the anatase-type crystal content is 70% or higher.
6. The titanium oxide sol as claimed in claim 4 , wherein the chlorine (Cl) content is 0.1 mass % or less.
7. The titanium oxide sol as claimed in claim 4 , wherein each content of carbon (C), sulfur (S), aluminum (Al), silicon (Si) and iron (Fe) is 0.01 mass % or less.
8. A method for producing ultrafine particulate titanium oxide, comprising drying the titanium oxide sol obtained by the method claimed in claim 1 .
9. Ultrafine particulate titanium oxide obtained by the method claimed in claim 8 .
10. A composition containing the titanium oxide claimed in claim 9 .
11. A material for solar cells containing the titanium oxide claimed in claim 9 .
12. A material for the electrode in lithium ion batteries containing the titanium oxide claimed in claim 9 .
13. A dielectric material containing the titanium oxide claimed in claim 9 .
14. The titanium oxide sol as claimed in claim 4 , wherein k is a value of 1 or more and less than 1.5.
15. The method for producing titanium oxide sol as claimed in claim 1 , which comprises mixing to completion an aqueous titanium tetrachloride solution into water at a temperature of 80° C. or higher within 30 seconds while maintaining the mixed solution at the temperature and cooling it to less than 60° C. within 15 minutes after the mixing is completed.
16. The method for producing titanium oxide sol as claimed in claim 1 , which comprises mixing to completion an aqueous titanium tetrachloride solution into water at a temperature of 80° C. or higher within not less than 5 seconds and not more than 30 seconds while maintaining the mixed solution at the temperature and cooling it to less than 60° C. within 15 minutes after the mixing is completed.