CA2551663A1 - Synthesis of ultrafine rutile phase titanium dioxide particles at low temperature - Google Patents
Synthesis of ultrafine rutile phase titanium dioxide particles at low temperature Download PDFInfo
- Publication number
- CA2551663A1 CA2551663A1 CA002551663A CA2551663A CA2551663A1 CA 2551663 A1 CA2551663 A1 CA 2551663A1 CA 002551663 A CA002551663 A CA 002551663A CA 2551663 A CA2551663 A CA 2551663A CA 2551663 A1 CA2551663 A1 CA 2551663A1
- Authority
- CA
- Canada
- Prior art keywords
- titanium dioxide
- ticl4
- phase
- range
- dopant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract 29
- 239000002245 particle Substances 0.000 title claims abstract 10
- 239000004408 titanium dioxide Substances 0.000 title claims abstract 9
- 230000015572 biosynthetic process Effects 0.000 title claims abstract 4
- 238000003786 synthesis reaction Methods 0.000 title claims abstract 4
- 238000000034 method Methods 0.000 claims abstract 22
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract 13
- 239000012071 phase Substances 0.000 claims abstract 9
- 239000012808 vapor phase Substances 0.000 claims abstract 5
- 230000007062 hydrolysis Effects 0.000 claims abstract 2
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract 2
- 229910003074 TiCl4 Inorganic materials 0.000 claims 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 9
- 239000000443 aerosol Substances 0.000 claims 7
- 239000002019 doping agent Substances 0.000 claims 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 6
- 239000000843 powder Substances 0.000 claims 6
- 239000000203 mixture Substances 0.000 claims 5
- 239000011261 inert gas Substances 0.000 claims 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 230000005587 bubbling Effects 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 2
- 230000003301 hydrolyzing effect Effects 0.000 claims 2
- 229910001026 inconel Inorganic materials 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- 229910052786 argon Inorganic materials 0.000 claims 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000001307 helium Substances 0.000 claims 1
- 229910052734 helium Inorganic materials 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- 229910052743 krypton Inorganic materials 0.000 claims 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 239000011541 reaction mixture Substances 0.000 claims 1
- 238000001089 thermophoresis Methods 0.000 claims 1
- 230000008016 vaporization Effects 0.000 claims 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nanotechnology (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a low temperature process for the synthesis of ultra rutile phase titanium dioxide particles through vapor phase hydrolysis of titanium tetra chloride.
Claims (21)
1. A process for synthesis of ultrafine rutile phase titanium dioxide particles through vapor phase hydrolysis of titanium tetrachloride comprising the step of:
(a) hydrolyzing a mixture of TiCl4 and H2O and a dopant in vapour phase in an aerosol reactor;
(b) collecting amorphous or anatase titanium dioxide powder formed as dry powders;
(c) calcining the dry powder to obtain rutile phase titanium dioxide.
(a) hydrolyzing a mixture of TiCl4 and H2O and a dopant in vapour phase in an aerosol reactor;
(b) collecting amorphous or anatase titanium dioxide powder formed as dry powders;
(c) calcining the dry powder to obtain rutile phase titanium dioxide.
2. A process as claimed in claim 1 wherein the amorphous particles of titanium dioxide are calcined at a temperature in the range of 150 to 400°C and for a period in the range of 1 to 4 hrs to generate rutile particles.
3. A process as claimed in claim 1 wherein the dopant contains a carbon atom and is selected from the group consisting of an aliphatic alcohol, an aromatic hydrocarbon, and any mixture thereof.
4. A process as claimed in claim 3 wherein the dopant is ethanol.
5. A process as claimed in claim 1 wherein the molar concentration of the dopant is 1 to based on the water vapour.
6. A process as claimed in claim 1 wherein the reaction mixture contains from 1 to 10 ethanol on a molar basis based on TiCl4.
7. A process as claimed in claim 1 wherein the flow rate of TiCl4 is in the range of 10 cm3/min to 200 cm3/min.
8. A process as claimed in claim 1 wherein the TiCl4 vapor concentration inside the reactor is in the range of 7 × 10-4mol/min to 1 × 10-2 mol/min.
9. A process as claimed in claim 1 wherein the flow rate of water vapour is in the range of 240 to 1500 cm3/min, preferably from 500 to 1000 cm3/min.
10. A process as claimed in claim 1 wherein the temperature at the exit of the aerosol reactor is maintained at less than 100°C for obtaining titanium dioxide particles having anatase phase.
11. A process as claimed in claim 1 wherein the aerosol reactor is externally heated in order to avoid particle coating on the walls through thermophoresis.
12. A process as claimed in claim 1 wherein the aerosol reactor comprises of 3 - tube concentric jet assembly wherein TiCl4 is introduced into the innermost tube, dopant is introduced into the outermost tube and water vapor is introduced into the middle tube.
13. A process as claimed in claim 12 wherein the 3-tube assembly comprises a concentric arrangement of three inconel tubes at the entrance of the aerosol reactor.
14. A process as claimed in claim 12 wherein vapor phase TiCl4 is introduced into a center tube of the three concentric inconel tubes.
15. A process as claimed in claim 1 wherein the vapor phase TiCl4 is formed by bubbling an inert gas through TiCl4 liquid.
16. A process as claimed in claim 1 wherein the inert gas is selected from the group consisting of argon, nitrogen, krypton, helium and any mixture thereof.
17. A process as claimed in claim 1 wherein the molar ratio of water to titanium tetra chloride in the feed is in the range 10 to 15.
18. A process as claimed in claim 1 wherein the water vapor is formed by bubbling air or inert gases through water under superheated condition.
19. A process as claimed in claim 1 wherein the reactor wall temperature is from 200 to 450°C.
20. A process as claimed in claim 1 wherein the rutile titanium dioxide particles formed have an average diameter in the range of from 25 to 150 nanometers.
21. A vapor phase process for the synthesis of ultrafine rutile titanium dioxide powders carried out in an aerosol reactor comprising the steps of:
(a) vaporizing a titanium chloride liquid, water and dopant such as ethanol separately for generating a reactant mixture;
(b) hydrolyzing TiCl4, H2O and dopant in vapour phase mixture in a continuous aerosol reactor under non-isothermal conditions at temperature in the range 80 to 135°C;
(c) collecting amorphous and anatase phase titanium dioxide powder as dry powder;
(d) calcining the titanium dioxide particles having the amorphous phase in the temperature ange of 150-400°C and time duration in the range of 1 to 4 hrs. to obtain titanium dioxide particles with rutile phase.
(a) vaporizing a titanium chloride liquid, water and dopant such as ethanol separately for generating a reactant mixture;
(b) hydrolyzing TiCl4, H2O and dopant in vapour phase mixture in a continuous aerosol reactor under non-isothermal conditions at temperature in the range 80 to 135°C;
(c) collecting amorphous and anatase phase titanium dioxide powder as dry powder;
(d) calcining the titanium dioxide particles having the amorphous phase in the temperature ange of 150-400°C and time duration in the range of 1 to 4 hrs. to obtain titanium dioxide particles with rutile phase.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/IN2003/000429 WO2005063629A1 (en) | 2003-12-31 | 2003-12-31 | Synthesis of ultrafine rutile phase titanium dioxide particles at low temperature |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2551663A1 true CA2551663A1 (en) | 2005-07-14 |
| CA2551663C CA2551663C (en) | 2010-03-23 |
Family
ID=34717550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2551663A Expired - Fee Related CA2551663C (en) | 2003-12-31 | 2003-12-31 | Synthesis of ultrafine rutile phase titanium dioxide particles at low temperature |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JP4800768B2 (en) |
| CN (1) | CN100532274C (en) |
| AU (1) | AU2003304660B2 (en) |
| CA (1) | CA2551663C (en) |
| DE (1) | DE10394356B4 (en) |
| GB (1) | GB2427860B (en) |
| WO (1) | WO2005063629A1 (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008519750A (en) * | 2004-11-11 | 2008-06-12 | バーゼル・ポリオレフィン・イタリア・ソチエタ・ア・レスポンサビリタ・リミタータ | Production of TiO2 powder from waste liquid containing titanium compound |
| WO2006051061A1 (en) * | 2004-11-11 | 2006-05-18 | Basell Poliolefine Italia S.R.L. | Preparation of tio2 powders from a waste liquid containing titanium compounds |
| EP1997781B1 (en) * | 2007-05-22 | 2014-07-16 | Evonik Degussa GmbH | Method for making titanium dioxide with variable sinter activity |
| US8609553B2 (en) | 2011-02-07 | 2013-12-17 | Micron Technology, Inc. | Methods of forming rutile titanium dioxide and associated methods of forming semiconductor structures |
| US8564095B2 (en) | 2011-02-07 | 2013-10-22 | Micron Technology, Inc. | Capacitors including a rutile titanium dioxide material and semiconductor devices incorporating same |
| JP5578572B2 (en) * | 2011-04-29 | 2014-08-27 | 独立行政法人産業技術総合研究所 | Composite particles |
| KR101290400B1 (en) | 2012-01-27 | 2013-07-26 | 군산대학교산학협력단 | Apparatus for preparing nano crystalline anatase titanium dioxide powder |
| CN103693687B (en) * | 2013-12-09 | 2015-06-24 | 云南新立有色金属有限公司 | Method and system for preparing titanium dioxide |
| KR101763357B1 (en) * | 2016-04-08 | 2017-08-01 | 케이씨 주식회사 | Preparation method of rutile titanium dioxide powder |
| CN109126894B (en) * | 2018-08-04 | 2021-07-23 | 山东迅达化工集团有限公司 | Preparation method of titanium dioxide carrier |
| CN109943103A (en) * | 2019-04-16 | 2019-06-28 | 正太新材料科技有限责任公司 | The preparation method and applications of rutile type titanium white |
| CN117410365A (en) * | 2023-12-15 | 2024-01-16 | 宁波长阳科技股份有限公司 | Solar cell module reflective film and preparation method and application thereof |
| CN117772172B (en) * | 2024-02-23 | 2024-05-03 | 山西安仑化工有限公司 | Preparation method and preparation device of titanium oxide/magnetic carbon black catalytic material |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS512440B1 (en) * | 1969-01-22 | 1976-01-26 | ||
| US4241042A (en) * | 1978-06-19 | 1980-12-23 | Montedison S.P.A. | Spherical titanium dioxide particles and process of manufacture |
| JPS59107905A (en) | 1982-12-09 | 1984-06-22 | Nippon Soda Co Ltd | Manufacture of hyperfine particle of metallic oxide |
| JPS59107904A (en) | 1982-12-09 | 1984-06-22 | Nippon Soda Co Ltd | Manufacture of fine particle of metallic oxide |
| IT1161200B (en) * | 1983-02-25 | 1987-03-18 | Montedison Spa | PROCESS AND APPARATUS FOR THE PREPARATION OF SINGLE-DISPERSED METAL OXIDE PARTICLES, SPHERICAL, NOT AGGREGATED AND OF LESS THAN MICRON |
| JP3170094B2 (en) * | 1993-04-08 | 2001-05-28 | 株式会社トクヤマ | Method for producing titanium oxide |
| US5698177A (en) * | 1994-08-31 | 1997-12-16 | University Of Cincinnati | Process for producing ceramic powders, especially titanium dioxide useful as a photocatalyst |
| PL187022B1 (en) * | 1996-07-25 | 2004-04-30 | Kerr Mcgee Chemical Llc | Method of and apparatus for obtaining titanium dioxide |
| KR100277164B1 (en) | 1998-07-16 | 2001-01-15 | 장인순 | A preparing method for crystalline micropowder of Titania from aqueous Titanium(Ⅳ) chloride by homogeneous precipitation process at low temperature |
| ATE445568T1 (en) * | 2000-03-29 | 2009-10-15 | Evonik Degussa Gmbh | DOPED TITANIUM DIOXIDE |
| JP4234298B2 (en) * | 2000-04-17 | 2009-03-04 | 東邦チタニウム株式会社 | Method for producing titanium oxide fine particles |
| KR100535358B1 (en) * | 2000-07-04 | 2005-12-09 | 비오이 하이디스 테크놀로지 주식회사 | Liquid crystal display device |
| JP4313535B2 (en) * | 2001-01-26 | 2009-08-12 | 昭和電工株式会社 | Fine particle titanium oxide composite, method for producing the composite, and composite composition |
-
2003
- 2003-12-31 CN CNB2003801109266A patent/CN100532274C/en not_active Expired - Fee Related
- 2003-12-31 JP JP2005512731A patent/JP4800768B2/en not_active Expired - Fee Related
- 2003-12-31 WO PCT/IN2003/000429 patent/WO2005063629A1/en not_active Ceased
- 2003-12-31 DE DE10394356.0T patent/DE10394356B4/en not_active Expired - Fee Related
- 2003-12-31 CA CA2551663A patent/CA2551663C/en not_active Expired - Fee Related
- 2003-12-31 AU AU2003304660A patent/AU2003304660B2/en not_active Ceased
- 2003-12-31 GB GB0614753A patent/GB2427860B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP4800768B2 (en) | 2011-10-26 |
| CN1886341A (en) | 2006-12-27 |
| WO2005063629A1 (en) | 2005-07-14 |
| DE10394356T5 (en) | 2007-04-12 |
| AU2003304660A1 (en) | 2005-07-21 |
| GB0614753D0 (en) | 2006-09-06 |
| AU2003304660B2 (en) | 2008-04-03 |
| GB2427860A (en) | 2007-01-10 |
| CN100532274C (en) | 2009-08-26 |
| GB2427860B (en) | 2009-03-25 |
| DE10394356B4 (en) | 2014-04-10 |
| JP2007527833A (en) | 2007-10-04 |
| CA2551663C (en) | 2010-03-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |
Effective date: 20180102 |