Concentrated photoactive, neutral titanium dioxide sol
View Patent ↗The present disclosure relates to methods of preparing sols of titanium dioxide nanoparticles that are photoactive, neutral, and in a substantially concentrated form. The methods particularly provide for concentrated sols in light of washing and dewatering under low cation concentrations and utilizing rapid peptizing through addition of the filter case to the peptizing agent. Concentrated acid may be utilized to maintain high TiO 2 concentration while still avoiding precipitation of the colloidal TiO 2 . Concentrated photoactive, neutral titanium dioxide sols are also provided as well as compositions thereof and photoactive coatings formed therewith.
1. A method for preparing a photocatalytic, neutral titanium dioxide sol, the method comprising:
washing and dewatering a hydrous titanium dioxide gel with an aqueous solvent having a cation concentration of about 500 ppm or less until achieving a filtrate conductivity of about 750 0 μS/cm or less and forming a titanium dioxide filter cake;
peptizing the titanium dioxide filter cake by adding the filter cake to an alkaline peptizing agent to provide a peptized alkaline titanium dioxide sol with a TiO 2 concentration of about 35% by weight or greater;
neutralizing the peptized alkaline titanium dioxide sol with a concentrated acid to provide a photocatalytic, neutral titanium dioxide sol with a pH of about 7 to about 9 and a TiO 2 concentration of about 30% by weight or greater.
2. The method according to claim 1 , wherein the washing and dewatering comprises processing the hydrous titanium dioxide gel in a filter press.
3. The method according to claim 1 , wherein the aqueous solvent is demineralized water.
4. The method according to claim 1 , wherein the aqueous solvent has a cation concentration of about 100 ppm or less.
5. The method according to claim 1 , wherein the aqueous solvent has a Ca 2+ concentration of about 50 ppm or less.
6. The method according to claim 1 , wherein the washing and dewatering is carried out until achieving a filtrate conductivity of about 600 0 μS/cm or less.
7. The method according to claim 1 , wherein the alkaline peptizing agent is selected from the group consisting of an alkylamine, a quaternary ammonium hydroxide, and combinations thereof.
8. The method according to claim 7 , wherein the alkaline peptizing agent is selected from the group consisting of diethylamine (DEA), tetraethyl ammonium hydroxide (TEAOH), and combinations thereof.
9. The method according to claim 1 , wherein the titanium dioxide filter cake is added under mixing.
10. The method according to claim 9 , wherein peptizing is substantially completed in a time of about 90 minutes or less.
11. The method according to claim 1 , wherein the peptized alkaline titanium dioxide sol has a TiO 2 concentration of about 40% by weight or greater.
12. The method according to claim 1 , wherein the peptized alkaline titanium dioxide sol has a pH of about 11 or greater.
13. The method according to claim 1 , wherein the concentrated acid comprises phosphoric acid.
14. The method according to claim 13 , wherein the phosphoric acid has a concentration of about 75% w/w or greater.
15. The method according to claim 1 , wherein the neutralizing is carried out in a time of about 120 minutes or less.
16. The method according to claim 1 , wherein the neutral titanium dioxide sol has a pH of about 8 to about 9 and a TiO 2 concentration of about 35% by weight or greater.
17. The method according to claim 1 , wherein the TiO 2 particles in the neutral titanium dioxide sol have an average size of about 50 nm or less.
18. The method according to claim 1 , wherein about 90% or greater of the TiO 2 particles in the neutral titanium dioxide sol are in the anatase form.
19. The method according to claim 1 , wherein the neutral titanium dioxide sol has a viscosity of about 40 centipoise to about 100 centipoise.
20. A method for preparing a photocatalytic, neutral titanium dioxide sol, the method comprising:
processing a hydrous titanium dioxide gel in a filter press with demineralized water having a Ca 2+ concentration of about 50 ppm or less until achieving a filtrate conductivity of about 500 0 μS/cm or less and forming a titanium dioxide filter cake;
peptizing the titanium dioxide filter cake by adding the filter cake to an alkaline peptizing agent with mixing to provide a peptized alkaline titanium dioxide sol with a TiO 2 concentration of about 35% by weight or greater, said peptizing being substantially completed in a time of about 60 minutes or less;
neutralizing the peptized alkaline titanium dioxide sol with phosphoric acid at a concentration of about 85% w/w or greater to provide a photocatalytic, neutral titanium dioxide sol with a pH of about 8 to about 9 and a TiO 2 concentration of about 35% by weight or greater.
21. The method of claim 1 , wherein the concentrated acid comprises phosphoric acid having a concentration of about 85% w/w or greater.
22. The method of claim 1 , further comprising, after the step of neutralizing the peptized alkaline titanium dioxide sol with a concentrated acid to provide a photocatalytic, neutral titanium dioxide sol with a pH of about 7 to about 9 and a TiO 2 concentration of about 30% by weight or greater, diluting said photocatalytic, neutral titanium dioxide sol with deionized water to provide a solution with a TiO 2 concentration of approximately 10% by weight based upon the total weight of said sol.
23. The method of claim 20 , further comprising, after the step of neutralizing the peptized alkaline titanium dioxide sol with phosphoric acid at a concentration of about 85% w/w or greater to provide a photocatalytic, neutral titanium dioxide sol with a pH of about 8 to about 9 and a TiO 2 concentration of about 35% by weight or greater, diluting said photocatalytic, neutral titanium dioxide sol with deionized water to provide a solution with a TiO 2 concentration of approximately 10% by weight based upon the total weight of said sol.
24. A method for preparing a photocatalytic, neutral titanium dioxide sol, the method comprising:
washing and dewatering a hydrous titanium dioxide gel with an aqueous solvent having a cation concentration of about 500 ppm or less until achieving a filtrate conductivity of about 750 μS/cm or less and forming a titanium dioxide filter cake;
peptizing the titanium dioxide filter cake by adding the filter cake to an alkaline peptizing agent to provide a peptized alkaline titanium dioxide sol with a TiO 2 concentration of about 35% by weight or greater;
neutralizing the peptized alkaline titanium dioxide sol with a concentrated acid, wherein said concentrated acid comprises phosphoric acid having a concentration of about 85% w/w or greater, to provide a photocatalytic, neutral titanium dioxide sol with a pH of about 7 to about 9 and a TiO 2 concentration of about 30% by weight or greater;
diluting said photocatalytic, neutral titanium dioxide sol with deionized water to provide a solution with a TiO 2 concentration of approximately 10% by weight based upon the total weight of said sol.