Visible light responsive doped titania photocatalytic nanoparticles and process for their synthesis

• US 9,352,302 B2
• Filed: 07/18/2014
• Issued: 05/31/2016
• Est. Priority Date: 07/20/2013
• Status: Active Grant

• Current Assignee: TATA Consultancy Services Limited (Tata Sons Pvt Ltd.)
• Original Assignee: TATA Consultancy Services Limited (Tata Sons Pvt Ltd.)
• Inventors: Maparu, Auhin Kumar, Rai, Beena
• Primary Examiner(s): Nguyen, Cam N.
• Application Number:
  US14/335,011
• Publication Number:
  US 20150024930A1
• Time in Patent Office: 683 Days
• Field of Search: 502/344, 502/347, 502/350
• US Class Current: 1/1
• CPC Class Codes: B01J 21/063 Titanium; Oxides or hydroxides thereof
• CPC Class Codes: B01J 23/50 Silver
• CPC Class Codes: B01J 23/52 Gold
• CPC Class Codes: B01J 35/30 characterised by their physical properties
• CPC Class Codes: B01J 35/39 Photocatalytic properties
• CPC Class Codes: B01J 35/40 characterised by dimensions, e.g. grain size in a colloidal state B01J35/23; crystallite size B01J35/77
• CPC Class Codes: B01J 37/0036 Grinding
• CPC Class Codes: B01J 37/009 Preparation by separation, e.g. by filtration, decantation, screening
• CPC Class Codes: B01J 37/32 Freeze drying, i.e. lyophilisation
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 23/047 Titanium dioxide
• CPC Class Codes: C01P 2002/52 containing elements as dopants
• CPC Class Codes: C01P 2002/54 one element only
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/84 by UV- or VIS- data
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/51 Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/52 highly monodisperse size distribution
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C09C 1/3623 Grinding

Abstract

Present disclosure provides a process for the synthesis of visible light responsive doped titania photocatalysts. The process involves step a) milling a mixture containing titania and a precursor compound, the compound selected from the group consisting of chloroauric acid and a mixture containing chloroauric acid and silver nitrate, in the presence of water and oxide milling media, at a temperature in the range of 20 to 50° C. for a period of 60-120 minutes, to form a slurry, wherein the amount of water is in the range of 15 to 25% by weight of the total mixture; and b) filtering the slurry to separate the oxide milling media and obtain a filtrate containing doped titania nanoparticles.

Claims

1. A process for the synthesis of visible light responsive doped titania photocatalytic nanoparticles, said process comprising the following steps:

a) milling a mixture, containing;

i) titania;

ii) a precursor compound, wherein the precursor compound is at least one selected from the group consisting of chloroauric acid and a mixture containing chloroauric acid and silver nitrate;

iii) water; and

iv) oxide milling media, wherein the oxide milling media consists of zirconia balls;

at a temperature in the range of 20 to 50°

C. for a period of 30-240 minutes, to form a slurry, wherein the amount of water is in the range of 15 to 25% by weight of the total mixture; and

b) filtering the slurry to separate the oxide milling media from the filtrate and further washing of the filtrate with water to obtain doped titania photocatalytic nanoparticles.

2. The process as claimed in claim 1, wherein the process further includes the step of drying the filtrate by any one of the methods selected from the group consisting of freeze drying, vacuum drying and air drying at low temperature.

3. The process as claimed in claim 1, wherein the ratio of precursor compound to titania particles is in the range of 1:

80 to 3;

80 w/w.

4. The process as claimed in claim 1, wherein the zirconia balls used is in the size range of 0.4-0.7 mm.

5. The process as claimed in claim 1, wherein the doped titania is a gold doped titania and the amount of gold atoms doped on titania surface is in the range of 0.5 to 0.7% by weight.

6. The process as claimed in claim 5, wherein the gold doped titania further comprises silver atoms on titania surface in the range of 0.02 to 0.07% by weight.

7. The process as claimed in claim 1, wherein the doped titania photocatalytic nanoparticles having particle size is in the range of 85-90 nm.

8. The process as claimed in claim 1, wherein the doped titania photocatalytic nanoparticles show no agglomeration.

9. Doped titania photocatalytic nanoparticles having particle size in the range of 85-90 nm, having photocatalytic activity under visible light irradiation, wherein the doped titania photocatalytic nanoparticles are gold doped titania and the amount of gold doped on the titania surface is in the range of 0.5-0.7% by weight.

10. The doped titania photocatalytic particles as claimed in claim 9, wherein the doped titania photocatalytic nanoparticles further comprises silver atoms on the titania surface and the amount of silver atoms on the titania surface is in the range of 0.02-0.07% by weight.