AU2003240024B2

Non-acidic, non-basic colloid solution containing dispersed titanium dioxide, method of manufacturing the same, and coating material comprising the colloid solution

Abstract

The present invention relates to a method of manufacturing a neutral and transparent titanium dioxide colloid solution wherein titanium dioxide nano particles is dispersed, and a novel titanium dioxide colloid solution prepared by the method. In addition, the present invention relates to a multifunctional, normal temperature curing-type coating agent comprising the titanium dioxide colloid solution.

Term

Term ended

Expired 30 May 2023, 3.3 years ago.

  1. Priority
  2. Filed
  3. Granted
  4. Expired
  5. Today

24 claims: 18 independent, 6 dependent

  1. 1
    Claims 1. A method of manufacturing a neutral and transparent water-based titanium dioxide colloid solution containing dispersed titanium dioxide nano particles, 5 comprising the following steps:(A) adding a titanium compound and a stabilizer to alcohol, wherein the said stabilizer is selected from the group consisting of an organic acid with alcohol group and ketone group, an organic acid with alcohol group and acetate group, and a salt thereof.;10 (B) slowly adding the reacted solution to distilled water while the solution is stirred;(C) neutralizing the resulting solution by adding a basic solution;and (D) heating the neutralized solution at a temperature of above 85 °C, wherein at step (A), the titanium compound and the stabilizer can be added in any 15 order.
  2. 3
    The method according to claims 1 or 2, characterized in that the alcohol is 20 added in the amount of 1 ~ 50% by weight, the stabilizer is added in the amount of at least 0.1% by weight based on the total solution, and the titanium compound is added in the amount of 1 ~ 5% by weight, which is calculated in terms of the amount of the T1O2 dispersed in the resultant titanium colloid solution, and the balance is water.
  3. 4
    The method according to claims 1 or 2, characterized in that the alcohol is 25 selected from the group consisting of lower alcohol having 1~ 4 carbon atoms such as methanol, ethanol, propanol, isopropanol or butanol.
  4. 5
    The method according to claims 1 or 2, characterized in that the titanium compound is selected from the group consisting of titanium(IV) isopropoxide (tetraisopropanol titanium), titanium(IV) butoxide, titanium(IV) ethoxide (titanium 30 tetraethanolate), titanium(IV) methoxide, titanium (IV) stearate and a mixture thereof.
  5. 6
    The method according to claims 1 or 2, characterized in that the stabilizer further comprises pentanediol, pentanedione, butanediol, butanedione, alkylacetoacetate, polyethylenglycol, cetyltrimethyl ammonium hydroxide, polyvinyl acetate, polyvinyl alcohol, trialkylalcohol amine((R0)3N), or a mixture thereof.
  6. 7
    The method according to claims 1 or 2, characterized in that the basic solution 5 is a solution of sodium hydroxide, a basic compound of alkaline metal, ammonium compound, an amine compound, a basic compound having an alkyl ammonium group, a basic compound of alkali earth metal, or a poly basic compound having a cationic ion such as aluminum ion.
  7. 8
    The method according to claims 1 or 2, characterized in that at step (A), in 10 addition to the titanium compound, an organic silicon compound, an aluminum compound, a zirconium compound, an iron compound or a mixture thereof is further added.
  8. 9
    The method according to claims 1 or 2, characterized in that the heating procedure of step (D) is replaced with a hydrothermal reaction being carried out at a 15 temperature of above 120 °C for 5 hrs in the high temperature, high pressure reactor.
  9. 10
    A method of manufacturing a neutral and transparent alcohol-based titanium dioxide colloid solution containing dispersed titanium dioxide nano particles, comprising the following steps:(a) adding a titanium compound and a stabilizer to alcohol, wherein the said 20 stabilizer is selected from the group consisting of an organic acid with alcohol group and ketone group, an organic acid with alcohol group and acetate group and a salt thereof;(b) neutralizing the resulting solution by adding a basic solution;and (c) heating the neutralized solution at a temperature of above 75 °C for more than 25 7 hrs, wherein at step (a), the titanium compound and the stabilizer can be added in any order.
  10. 12
    The method according to claims 10 or 11, characterized in that the alcohol is added in the amount of 50 ~ 90% by weight, the stabilizer be added in the amount of at least 0.1% by weight based on the total solution, and the titanium dioxide compound be added in the amount of 1 ~ 5% by weight, which is calculated in terms of the amount of TiO 2 dispersed in the resultant titanium colloid solution, and the balance is water. '
  11. 13
    The method according to claims 10 or 11, characterized in that the alcohol is selected from the group consisting of lower alcohol having 1~ 4 of carbon atoms such as methanol, ethanol, propanol, isopropanol or butanol.
  12. 14
    The method according to claims 10 or 11, characterized in that the titanium compound is selected from the group consisting of titanium(IV) isopropoxide (tetraisopropanol titanium), titanium(IV) butoxide, titanium(IV) ethoxide (titanium tetraethanolate), titanium(IV) methoxide, titanium(IV) stearate and a mixture thereof.
  13. 15
    The method according to claims 10 or 11, characterized in that the stabilizer further comprises pentanediol, pentanedione, butanediol, butanedione, alkylacetoacetate, polyethylenglycol, cetyltrimethyl ammonium hydroxide, polyvinyl acetate, polyvinyl alcohol, trialkylalcohol amine((R0)3N), or a mixture thereof.
  14. 16
    The method according to claims 10 or 11, characterized in that the basic solution is a soultion of sodium hydroxide, basic compound of alkaline metal, ammonium compound, amine compound, basic compound having an alkyl ammonium group, basic compound of alkali earth metal, or poly basic compound having a cationic ion such as aluminum ion.
  15. 17
    The method according to claims 10 or 11, characterized in that at step (A), in addition to the titanium compound, an organic silicon compound, an aluminum compound, a zirconium compound, an iron compound or a mixture thereof is further added.
  16. 18
    The method according to claims 10 or 11, characterized in that the heating procedure of step (c) is replaced with a hydrothermal reaction being carried out at a temperature of above 120 °C for 5 hrs in the high temperature, high pressure reactor.
  17. 19
    A neutral and transparent titanium dioxide colloid solution prepared by the method according to any one of claims 1 to 18, wherein 1 ~ 5 % by weight of titanium dioxide nano particles of anatase structure is dispersed.
  18. 22
    A neutral, transparent, water-based or alcohol-based composition, wherein 1-5% by weight of TiCty is dispersed, and comprises at least 0.1% by weight of a stabilizer selected from the group consisting of glycolic acid, pentanediol, pentanedione, butanediol, butanedione, aqueous glycolic salt solution and a mixture thereof;a basic solution in the amount capable of neutralizing the stabilizer;and the balance of water or alcohol as a solvent.
  19. 24
    The composition according to claims 22 or 23, further comprises an organic silicon compound, an aluminum compound, a zirconium compound, an iron compound or a mixture thereof. 1/4 Figi Absorbance 2/4 Fig 3 Wavelength (nm) Relative Intensity Fig 4 2Θ 3/4 Fig 5 Fig 6 4/4 Fig 7
Independent claims19