CN1351962A - Low temperature processing of preparing nanometer rutile phase titanium dioxide - Google Patents
Low temperature processing of preparing nanometer rutile phase titanium dioxide Download PDFInfo
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- CN1351962A CN1351962A CN 01140101 CN01140101A CN1351962A CN 1351962 A CN1351962 A CN 1351962A CN 01140101 CN01140101 CN 01140101 CN 01140101 A CN01140101 A CN 01140101A CN 1351962 A CN1351962 A CN 1351962A
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Abstract
A low temperature process of preparing nanometer rutile phase titania includes compounding reaction solution A with tetrabutyl titanate and ethanol, compounding reaction solution B with deionized water and nitric acid, adding solution A slowly into solution B and stirring to form a uniform solution, further stirring at room temperature for complete hydrolysis to become a sol, maintaining the sol at 30-60 deg.C for 5-20 hr to convert into gel gradually, and then becoming powder, that is the requried nanometer rutile phase titania. The process of the present inventino is simple, easy to operate, low in power preparing temperature, saving in power, pollution-less, high in product purity and homogeneous in product particle.
Description
Technical field
The present invention relates to the method that a kind of low temperature prepares the nanometer rutile phase titanic oxide, belong to field of fine chemical.
Background technology
Titanium dioxide is very stable weak intermediate oxide, reacts with other element and compound hardly under the room temperature, is insoluble in water, lipid acid, other organism and diluted mineral acid (except the HF).Titanium dioxide because have that specific refractory power height, whiteness are good, opacifying power and premium propertiess such as strong coloring force, gloss and good dispersity, resistance to chemical attack, thermostability and uvioresistant, be widely used in fields such as coating, printing paint, papermaking, plastic, rubber.Titanium dioxide can also be done catalyzer, sorbent material, and can be used for sterilization and sewage treatment area.Red schorl phase titanium dioxide is widely used in aspects such as senior pigment, makeup, and its tinting strength is better than anatase octahedrite, is 8 times of the white pigment lithopone used always.In electronic industry, red schorl phase titanium dioxide is used to make electrical condenser, piezoelectric device and transparent photoelectric pottery owing to have very high specific inductivity and resistance.
Nano titanium oxide has been inherited the advantage of ordinary titanium dioxide, simultaneously since the particulate yardstick between molecule, atom and bulk material, its surface electronic structure and crystalline structure change, produce the surface effects that bulk material did not have, quantum effect etc., made nano titanium dioxide powder and conventional titanium dioxide relatively have a series of special physicochemical character.Have a wide range of applications.
In disclosed known technology, the method for preparing the nanometer rutile phase titanic oxide has following several.Chinese patent CN1217297 is a raw material with titanium sulfate, titanyl sulfate or metatitanic acid, through precipitation, coats, and 500-650 ℃ of calcination, dissolving then also needs 800-900 ℃ to carry out the crystal formation conversion at last.This complicated process of preparation needs high-temperature calcination just can obtain red schorl phase titanium dioxide, and the titanium dioxide purity that makes is low.Chinese patent CN1114949 is a main raw material with ilmenite and technical hydrochloric acid, produce certain density metatitanic acid after, add two kinds of organism and carry out atmospheric hot-water and separate, can make the nanometer rutile phase titanic oxide.This method technology is complicated, and also needs calcining just can obtain product.CN12488550 utilizes titanium tetrachloride to be main raw material, adopts mineral acid control hydrolysis velocity, and precipitation after the vacuum-drying, can make the red schorl phase titanium dioxide that particle diameter is 7-100nm after washing, alcohol are washed.Though this method at room temperature promptly can make the nanometer rutile phase titanic oxide, because the titanium tetrachloride volatility is extremely strong, the difficulty of concrete operations is bigger, easily contaminate environment.
Summary of the invention
The objective of the invention is to propose the method that a kind of low temperature prepares the nanometer rutile phase titanic oxide, overcome the shortcoming of prior art, simplify preparation technology, avoid environmental pollution, and handle acquisition nanometer rutile phase titanic oxide with lesser temps.
The low temperature that the present invention proposes prepares the method for nanometer rutile phase titanic oxide, comprises following each step:
1, tetrabutyl titanate and ethanol are made into reaction soln A, deionized water and nitric acid are made into reaction soln B, then solution A is slowly added in the solution B, make the mol ratio of each composition in the solution be: tetrabutyl titanate: ethanol: nitric acid: water=1: 0～15: 0.05～4: 10～100;
2, above-mentioned solution stirring is become homogeneous solution, at room temperature continue to stir 10～50min again, making it complete hydrolysis becomes colloidal sol;
3, with colloidal sol in 30～60 ℃ the insulation 5～20 hours, colloidal sol gradually becomes gel, becomes powder at last, promptly obtains the nanometer rutile phase titanic oxide.
In order to make the titanium dioxide crystalline form complete, the powder that can make above-mentioned the 4th step obtains well-crystallized's nanometer rutile phase titanic oxide at last in 200～600 ℃ of calcinings 1～3 hour.
The low temperature that the present invention proposes prepares the method for nanometer rutile phase titanic oxide, and preparation technology is simple, easy handling, and the synthesis temperature of powder is lower, thereby can save the energy, and pollution-free, the purity height of product, uniform particles.
Embodiment
Embodiment 1
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 0.05: 10, in stirring at room 10min, making it complete hydrolysis becomes colloidal sol with solution.In 60 ℃ of insulations 5 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 200 ℃ of calcinings 1 hour, is promptly obtained nanometer rutile phase titanic oxide (50nm).
Embodiment 2
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 0.1: 20, in stirring at room 20min, making it complete hydrolysis becomes colloidal sol with solution.In 50 ℃ of insulations 8 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 300 ℃ of calcinings 2 hours, is promptly obtained nanometer rutile phase titanic oxide (40nm).
Embodiment 3
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 0.3: 30, in stirring at room 30min, making it complete hydrolysis becomes colloidal sol with solution.In 40 ℃ of insulations 12 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 400 ℃ of calcinings 1 hour, is promptly obtained nanometer rutile phase titanic oxide (80nm).
Embodiment 4
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 2: 40, in stirring at room 40min, making it complete hydrolysis becomes colloidal sol with solution.In 45 ℃ of insulations 10 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 450 ℃ of calcinings 1 hour, is promptly obtained nanometer rutile phase titanic oxide (40nm).
Embodiment 5
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 3: 50, in stirring at room 50min, making it complete hydrolysis becomes colloidal sol with solution.In 50 ℃ of insulations 10 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 500 ℃ of calcinings 1 hour, is promptly obtained nanometer rutile phase titanic oxide (55nm).
Embodiment 6
Deionized water and nitric acid are made into reaction soln B, tetrabutyl titanate is slowly added in the solution B, stirring becomes homogeneous solution, tetrabutyl titanate in the solution: nitric acid: water=1: 4: 100, in stirring at room 60min, making it complete hydrolysis becomes colloidal sol with solution.In 45 ℃ of insulations 18 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 500 ℃ of calcinings 1.5 hours, is promptly obtained nanometer rutile phase titanic oxide (50nm).
Embodiment 7
With tetrabutyl titanate and alcohol solution-forming A, deionized water and nitric acid are made into reaction soln B.Solution A is slowly added in the solution B, and stirring becomes homogeneous solution, tetrabutyl titanate in the solution: ethanol: nitric acid: water=1: 2: 1: 40, and in stirring at room 30min, making it complete hydrolysis becomes colloidal sol with solution.In 60 ℃ of insulations 6 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder was promptly obtained nanometer rutile phase titanic oxide (70nm) in 2 hours in 600 ℃ of calcinings.
Embodiment 8
With tetrabutyl titanate and alcohol solution-forming A, deionized water and nitric acid are made into reaction soln B.Solution A is slowly added in the solution B, and stirring becomes homogeneous solution, tetrabutyl titanate in the solution: ethanol: nitric acid: water=1: 5: 2.5: 60, and in stirring at room 50min, making it complete hydrolysis becomes colloidal sol with solution.In 50 ℃ of insulations 10 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 600 ℃ of calcinings 3 hours, is promptly obtained nanometer rutile phase titanic oxide (80nm).
Embodiment 9
With tetrabutyl titanate and alcohol solution-forming A, deionized water and nitric acid are made into reaction soln B.Solution A is slowly added in the solution B, and stirring becomes homogeneous solution, tetrabutyl titanate in the solution: ethanol: nitric acid: water=1: 10: 0.5: 30, and in stirring at room 30min, making it complete hydrolysis becomes colloidal sol with solution.In 40 ℃ of insulations 14 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 600 ℃ of calcinings 3 hours, is promptly obtained nanometer rutile phase titanic oxide (50nm).
Embodiment 10
With tetrabutyl titanate and alcohol solution-forming A, deionized water and nitric acid are made into reaction soln B.Solution A is slowly added in the solution B, and stirring becomes homogeneous solution, tetrabutyl titanate in the solution: ethanol: nitric acid; Water=1: 15: 1.5: 40, in stirring at room 30min, making it complete hydrolysis becomes colloidal sol with solution.In 30 ℃ of insulations 20 hours, colloidal sol gradually became gel, becomes powder at last with colloidal sol, and powder in 600 ℃ of calcinings 3 hours, is promptly obtained nanometer rutile phase titanic oxide (65nm).
Claims (2)
1, a kind of low temperature prepares the method for nanometer rutile phase titanic oxide, it is characterized in that this method comprises following each step:
(1) tetrabutyl titanate and ethanol are made into reaction soln A, deionized water and nitric acid are made into reaction soln B, then solution A is slowly added in the solution B, make the mol ratio of each composition in the solution be: tetrabutyl titanate: ethanol: nitric acid: water=1: 0～15: 0.05～4: 10～100;
(2) above-mentioned solution stirring becomes homogeneous solution, at room temperature continues to stir 10～50min again, and making it complete hydrolysis becomes colloidal sol;
(3) with colloidal sol in 30～60 ℃ the insulation 5～20 hours, colloidal sol gradually becomes gel, becomes powder at last, promptly obtains the nanometer rutile phase titanic oxide.
2, the method for claim 1 is characterized in that also comprising that the powder that described the 4th step is made in 200～600 ℃ of calcinings 1～3 hour, obtains well-crystallized's nanometer rutile phase titanic oxide at last.
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| CN 01140101 CN1131173C (en) | 2001-11-23 | 2001-11-23 | Low temperature processing of preparing nanometer rutile phase titanium dioxide |
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| CN 01140101 CN1131173C (en) | 2001-11-23 | 2001-11-23 | Low temperature processing of preparing nanometer rutile phase titanium dioxide |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100392023C (en) * | 2005-09-01 | 2008-06-04 | 江苏大学 | Nanometer rutile titania sedimentation for preparing mica titanium nanometer composite material |
| CN100424020C (en) * | 2006-11-23 | 2008-10-08 | 上海交通大学 | Low temperature method for preparing Nano powder |
| CN101385967B (en) * | 2008-10-15 | 2010-08-25 | 张家港市普生光电有限公司 | Preparation method of nano titanic oxide film for photochemical catalyst |
| CN101456583B (en) * | 2007-12-12 | 2011-05-25 | 中国科学院理化技术研究所 | Synthetic method for preparing rutile type nano titanic oxide sol or powder at low temperature |
| CN101671052B (en) * | 2009-09-08 | 2011-06-08 | 西安瑞联近代电子材料有限责任公司 | Method for preparing anatase-shaped nano TiO2 |
| CN102433978A (en) * | 2011-09-07 | 2012-05-02 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102587610A (en) * | 2012-01-31 | 2012-07-18 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN102658103A (en) * | 2012-04-17 | 2012-09-12 | 太原理工大学 | Preparation method and application of high-active-dispersibility nanometer titanium dioxide |
| CN102674452A (en) * | 2012-05-23 | 2012-09-19 | 沈阳化工大学 | Method for preparing nano titanium dioxide by sol process at low temperature |
| CN102730754A (en) * | 2012-06-07 | 2012-10-17 | 江苏恒智纳米科技有限公司 | Preparation method of aqueous nano-TiO2 colloid |
| CN105645951A (en) * | 2016-01-06 | 2016-06-08 | 昆明理工大学 | Method for promoting phase change of titanium dioxide and inhibiting grain growth |
| CN106883662A (en) * | 2017-01-24 | 2017-06-23 | 东北大学秦皇岛分校 | A kind of coating polymolecularity TiO2Filler and preparation method thereof |
| CN111607210A (en) * | 2020-05-28 | 2020-09-01 | 宁波德伟电器有限公司 | PC flame-retardant composite material for household appliances and preparation method thereof |
| CN112694122A (en) * | 2020-12-14 | 2021-04-23 | 浙江大学温州研究院 | Preparation method of granular titanium dioxide sol |
-
2001
- 2001-11-23 CN CN 01140101 patent/CN1131173C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100392023C (en) * | 2005-09-01 | 2008-06-04 | 江苏大学 | Nanometer rutile titania sedimentation for preparing mica titanium nanometer composite material |
| CN100424020C (en) * | 2006-11-23 | 2008-10-08 | 上海交通大学 | Low temperature method for preparing Nano powder |
| CN101456583B (en) * | 2007-12-12 | 2011-05-25 | 中国科学院理化技术研究所 | Synthetic method for preparing rutile type nano titanic oxide sol or powder at low temperature |
| CN101385967B (en) * | 2008-10-15 | 2010-08-25 | 张家港市普生光电有限公司 | Preparation method of nano titanic oxide film for photochemical catalyst |
| CN101671052B (en) * | 2009-09-08 | 2011-06-08 | 西安瑞联近代电子材料有限责任公司 | Method for preparing anatase-shaped nano TiO2 |
| CN102433978A (en) * | 2011-09-07 | 2012-05-02 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102433978B (en) * | 2011-09-07 | 2015-05-20 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102587610B (en) * | 2012-01-31 | 2014-10-29 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN102587610A (en) * | 2012-01-31 | 2012-07-18 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN102658103A (en) * | 2012-04-17 | 2012-09-12 | 太原理工大学 | Preparation method and application of high-active-dispersibility nanometer titanium dioxide |
| CN102674452A (en) * | 2012-05-23 | 2012-09-19 | 沈阳化工大学 | Method for preparing nano titanium dioxide by sol process at low temperature |
| CN102730754A (en) * | 2012-06-07 | 2012-10-17 | 江苏恒智纳米科技有限公司 | Preparation method of aqueous nano-TiO2 colloid |
| CN105645951A (en) * | 2016-01-06 | 2016-06-08 | 昆明理工大学 | Method for promoting phase change of titanium dioxide and inhibiting grain growth |
| CN106883662A (en) * | 2017-01-24 | 2017-06-23 | 东北大学秦皇岛分校 | A kind of coating polymolecularity TiO2Filler and preparation method thereof |
| CN111607210A (en) * | 2020-05-28 | 2020-09-01 | 宁波德伟电器有限公司 | PC flame-retardant composite material for household appliances and preparation method thereof |
| CN112694122A (en) * | 2020-12-14 | 2021-04-23 | 浙江大学温州研究院 | Preparation method of granular titanium dioxide sol |
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