# US 7,611,688 B2 · Rutile titania nano sols and process for manufacturing the same

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- Number: US 7,611,688 B2
- Document ID: US7611688B2
- Status: Granted
- Kind: B2
- Application number: 11/209,412
- Filed: 2005-08-23
- Published: 2006-05-25
- Granted: 2009-11-03
- Earliest claimed: 2004-11-19
- Assignees: Korea Research Institute of Chemical Technology
- Inventors: Sang-Il Seok; Bok-Yeop Ahn; Hoon Kim
- Web page: https://patentgrep.com/patent/US7611688B2

## CPC

- C01G 23/053: Producing by wet processes, e.g. hydrolysing titanium salts
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/80: Compositional purity
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention is related to a process of manufacturing rutile high-purity titania nano sols in a pure aqueous medium having no ionic impurities. In more detail, the present invention is related to a process for manufacturing titania nano sols, in which high-purity rutile titania nano particles are dispersed stably, through the hydrolysis of titanium tetraisopropoxide in an aqueous solution containing hydrogen peroxide (H2O2), and simultaneously with the hydrolysis, formation of peroxotitanate precursors, and hydrothermal treatment of them at 50-120° C.

## Claims

### Claim 1

A process for manufacturing water-dispersible rutile nano sol particles consisting of titania, comprising the steps of:
i) manufacture of a mixed solvent consisting of water and hydrogen peroxide; wherein a mole ratio of water to hydrogen peroxide is 10-20;
ii) having hydrolysis and the formation of peroxotitanate occur simultaneously by dropping down titanium tetraisopropoxide to said mixed solvent of water and hydrogen peroxide, wherein a mole ratio of titanium tetraisopropoxide to hydrogen peroxide is 0.01-0.03; and
iii) hydrothermal treatment at 90-120° C. for 3-24 hours of an aqueous solution in which said peroxotitanate is dissolved,
wherein the steps i), ii) and iii) are performed in that order.

### Claim 2 (depends on 1)

The process for manufacturing water-dispersible rutile nano sol particles consisting of titania of claim 1, characterized by that the purity of said water-dispersible rutile nano sol particles consisting of titania is greater than 99.99%, wherein said purity is based on the intensity ratio of peak of the rutile nano sol particles consisting of titania in X-ray difffractometry.