CN1958460A - Low temperature method for preparing Nano powder - Google Patents
Low temperature method for preparing Nano powder Download PDFInfo
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Abstract
This invention relates to a low-temperature method for preparing TiO2 nanopowder. The method comprises: utilizing tetrabutyl titanate as the precursor, dropping into ice water solution containing acid to prepare TiO2 hydrosol, drying at room temperature, and drying at 120-180 deg.C to obtain anatase-type TiO2 nanopowder. This invention utilizes low temperature method, and only adopts aqueous solution of diluted acid as the sovent, thus avoiding alcohol or other stabilizers. The method has such advantages as simple process, low energy consumption and little pollution. The obtained TiO2 nanopowder has large specific surface area and high photocatalytic activity. By rational combination of carrier and UV source, the TiO2 nanopowder can effectively remove organic pollutants.
Description
Technical field
The present invention relates to a kind of TiO
2The preparation method of nano-powder, particularly a kind of TiO
2The low temperature preparation method of nano-powder belongs to the environmental purification technical field.
Technical background
Photochemical catalysis is a kind of emerging environmental purification technology.Nano-TiO
2Photocatalyst oxidation or reduction effectively is adsorbed on its lip-deep obnoxious flavour molecule, and kill bacteria suppresses virus, and harmful organic substance, bacterium etc. can be converted into innoxious substances such as water and carbonic acid gas, and without any secondary pollution.The photocatalyst of existing preparation is TiO mostly
2Nano-powder is in order to improve TiO
2Photocatalytic activity, must make it have higher degree of crystallinity, smaller particles size and higher specific surface area so that there is more chain carrier to participate in reaction, increase active.At various preparation TiO
2In the method for nano-powder, sol-gel method is widely adopted, and is easy and simple to handle because this method has the equipment less investment, multiple advantages such as easy controlled doping.Usually adopt the TiO of sol gel process preparation at normal temperatures
2Powder is not if carry out high-temperature heat treatment, TiO
2Be non-crystalline state, show any photocatalytic activity hardly, and the sol gel process majority to make solvent with alcohol, also will add stablizer with control hydrolysis.Will be with TiO
2Be transformed into the anatase octahedrite phase of crystalline state from non-crystalline state, it at high temperature must be heat-treated.But the raising of thermal treatment temp will cause particle to be grown up and specific surface area descends.The TiO that has the low particle size of high specific surface area for acquisition
2Nano-photocatalyst, the low temperature preparation is an approach that addresses this problem.
Find through literature search prior art, the Chinese invention patent application number is 200610059353.4, name is called: the low temperature preparation method of nano meso-porous titanium dioxide, it is the presoma of preparation nano titanium oxide that this technology discloses with titanate and dehydrated alcohol, at first that tetrabutyl titanate and dehydrated alcohol is mixed, again acid solution is added wherein, it is left standstill curing, dry and obtain xerogel, again the gel powder is put into the ethanolic soln of acid after levigate, made titanium dioxide by the unformed titanium dioxide that changes crystalline phase into after the stirring and refluxing of heating back.But the preparation of the presoma of the nano titanium oxide that this technology is related needs alcohol to make solvent, also need add template, and required medicine is more, and the preparation method is more loaded down with trivial details.
Summary of the invention
In order to overcome the deficiency of above technical problem, the invention provides a kind of TiO
2The low temperature preparation method of nano-powder passes through to TiO it
2The preparation method's of nano-powder improvement reaches the purpose that improves photocatalysis efficiency.
The present invention is achieved by the following technical solutions:
The present invention, is added drop-wise in the acidiferous frozen water solution and prepares TiO as presoma with tetrabutyl titanate
2The water-sol, after drying at room temperature, make TiO through 120-180 ℃ of oven dry again with anatase crystal
2Nano-powder.
Described preparation TiO
2The water-sol, be specially: under magnetic agitation, dropwise adding tetrabutyl titanate lentamente in containing nitric acid or hydrochloric frozen water solution, stirred 24-48 hour under the room temperature, the upper strata is the butanols that hydrolysis produces behind the solution left standstill, and lower floor is transparent titania hydrosol, separates to obtain TiO
2The water-sol.The volumetric molar concentration of nitric acid or hydrochloric acid is 0.05～0.15mol/L in the used acidiferous frozen water solution, and the volumetric molar concentration of tetrabutyl titanate is 0.2～1mol/L in the titania hydrosol of making.
The present invention is in order to reduce TiO
2Particle grain size improves TiO
2Specific surface area, improve the activity of photocatalytic activity component, after having prepared the water-sol with the tetrabutyl titanate for presoma low temperature, the water-sol makes TiO through oven drying at low temperature again through drying at room temperature
2Nano-powder, its bake out temperature are 120-180 ℃, and drying time is 180 minutes.The TiO that process low temperature prepares
2Nano-powder, photocatalytic activity height and preparation process are easy, less energy consumption, cost is low.
The present invention is the presoma of colloidal sol with cheap tetrabutyl titanate, adopts sol-gel method, only with the aqueous solution of diluted acid, need not make solvent by alcohol, and not add other stablizers, and low temperature synthesizes TiO
2The water-sol, drying at room temperature, oven drying at low temperature, preparation TiO
2Nano-powder, having solved common sol-gel method effectively needs heat and causes TiO
2The problem that the nano-photocatalyst particle is grown up and specific surface area descends, and energy efficient, preparation technology is very easy.
The present invention has substantive distinguishing features and significance progress, the present invention is owing to adopt low-temperature fabrication, its preparation technology is easy, energy-conserving and environment-protective and photocatalytic activity ratio of component surface-area are big, the photocatalytic activity height, by configuration suitable carriers and ultraviolet source, can remove organic pollutant effectively.
Embodiment
In conjunction with content of the present invention, provide following examples:
Embodiment 1:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of nitric acid stirred 24 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of nitric acid is for O.05mol/L in the frozen water solution of used nitric acid, and the volumetric molar concentration of tetrabutyl titanate is 0.2mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 120 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 144.2m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches 60% to the degradation rate of acetaldehyde.
Embodiment 2:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of nitric acid stirred 36 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of nitric acid is 0.1mol/L in the frozen water solution of used nitric acid, and the volumetric molar concentration of tetrabutyl titanate is 0.6mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 150 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 153.1m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches 67% to the degradation rate of acetaldehyde.
Embodiment 3:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of nitric acid stirred 48 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of nitric acid is 0.15mol/L in the frozen water solution of used nitric acid, and the volumetric molar concentration of tetrabutyl titanate is 1mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 180 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 167.3m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches 71% to the degradation rate of acetaldehyde.
Embodiment 4:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of hydrochloric acid stirred 24 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of hydrochloric acid is 0.05mol/L in the frozen water solution of used hydrochloric acid, and the volumetric molar concentration of tetrabutyl titanate is 0.2mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 120 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 147.3m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches about 60% the degradation rate of acetaldehyde.
Embodiment 5:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of hydrochloric acid stirred 36 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of hydrochloric acid is 0.1mol/L in the frozen water solution of used hydrochloric acid, and the volumetric molar concentration of tetrabutyl titanate is 0.6mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 150 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 157.6m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches 63% to the degradation rate of acetaldehyde.
Embodiment 6:
1, under the magnetic agitation, dropwise adding tetrabutyl titanate lentamente in the frozen water solution of hydrochloric acid stirred 48 hours under the room temperature, layering behind the solution left standstill, upper strata are the butanols that hydrolysis produces, and lower floor is transparent titania hydrosol, its separatory is obtained titania hydrosol, stand-by.The volumetric molar concentration of hydrochloric acid is 0.15mol/L in the frozen water solution of used hydrochloric acid, and the volumetric molar concentration of tetrabutyl titanate is 1mol/L in the titania hydrosol;
2, with above-mentioned titania hydrosol drying at room temperature, grind, put into 180 ℃ of oven dry of baking oven 3 hours, promptly make TiO
2Nano-powder, specific surface area are 170m
2/ g;
3, the TiO of low temperature preparation
2Nano-powder is used the degradation rate test shows to the high density aldehydes gas, and this powder reaches 70% to the degradation rate of acetaldehyde.
Claims (5)
1, a kind of TiO
2The low temperature preparation method of nano-powder is characterized in that,, is added drop-wise in the acidiferous frozen water solution and prepares TiO as presoma with tetrabutyl titanate
2The water-sol, after drying at room temperature, make TiO through 120-180 ℃ of oven dry again with anatase crystal
2Nano-powder.
2, TiO according to claim 1
2The low temperature preparation method of nano-powder is characterized in that, described preparation TiO
2The water-sol, be specially: under magnetic agitation, dropwise adding tetrabutyl titanate lentamente in containing nitric acid or hydrochloric frozen water solution stirs under the room temperature, and the upper strata is the butanols that hydrolysis produces behind the solution left standstill, and lower floor is transparent titania hydrosol, separates to obtain TiO
2The water-sol.
3, TiO according to claim 2
2The low temperature preparation method of nano-powder is characterized in that, stirs under the described room temperature, and churning time is 24-48 hour.
4, TiO according to claim 2
2The low temperature preparation method of nano-powder is characterized in that, the volumetric molar concentration of nitric acid or hydrochloric acid is 0.05～0.15mol/L in the described acidiferous frozen water solution.
5, TiO according to claim 2
2The low temperature preparation method of nano-powder is characterized in that, the volumetric molar concentration of described tetrabutyl titanate in titania hydrosol is 0.2～1mol/L.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103962119A (en) * | 2014-05-17 | 2014-08-06 | 天津微能新材料有限公司 | Preparation method of TiO2 photocatalyst mesh and TiO2 photocatalyst mesh |
| CN105289620A (en) * | 2015-11-23 | 2016-02-03 | 哈尔滨工业大学 | Method for preparing catalyst for adsorption and degradation of organic pollutants in waste water |
| CN105551828A (en) * | 2015-12-11 | 2016-05-04 | 郑州大学 | Nano titanium dioxide/graphene composite material and preparation method thereof |
| CN105664808A (en) * | 2016-01-13 | 2016-06-15 | 云南大学 | Method for preparing stable nano anatase titanium dioxide alcohol phase sol at low temperature |
| CN107799756A (en) * | 2017-10-31 | 2018-03-13 | 湘潭大学 | A kind of Na2Ti3O7The preparation method of C nano fiber |
| CN107915254A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of nano-titanium dioxide powder |
| CN107915252A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of nano-titanium dioxide powder |
| CN107913693A (en) * | 2017-11-23 | 2018-04-17 | 中国科学院福建物质结构研究所 | The oxygen-enriched state titanium oxide in surface and preparation method for high-activity treatment of textile dye waste |
| CN107913692A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of TiO 2 sol |
| CN110668496A (en) * | 2019-11-14 | 2020-01-10 | 大连交通大学 | Method for preparing rutile TiO by HCl volatilization low-temperature method2Nano powder |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324767A (en) * | 2001-07-12 | 2001-12-05 | 张汝冰 | Low temperature prepn. of rutile type nanometer titania by using titanic acid as raw material |
| CN1131173C (en) * | 2001-11-23 | 2003-12-17 | 清华大学 | Low temperature processing of preparing nanometer rutile phase titanium dioxide |
| CN1197780C (en) * | 2002-10-23 | 2005-04-20 | 中国科学院化学研究所 | Low temperature preparing process for anatase phase nano crystal titanium dioxide of light catalystic activity |
-
2006
- 2006-11-23 CN CNB2006101186681A patent/CN100424020C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103962119A (en) * | 2014-05-17 | 2014-08-06 | 天津微能新材料有限公司 | Preparation method of TiO2 photocatalyst mesh and TiO2 photocatalyst mesh |
| CN105289620A (en) * | 2015-11-23 | 2016-02-03 | 哈尔滨工业大学 | Method for preparing catalyst for adsorption and degradation of organic pollutants in waste water |
| CN105551828A (en) * | 2015-12-11 | 2016-05-04 | 郑州大学 | Nano titanium dioxide/graphene composite material and preparation method thereof |
| CN105664808A (en) * | 2016-01-13 | 2016-06-15 | 云南大学 | Method for preparing stable nano anatase titanium dioxide alcohol phase sol at low temperature |
| CN107915252A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of nano-titanium dioxide powder |
| CN107915254A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of nano-titanium dioxide powder |
| CN107913692A (en) * | 2016-10-08 | 2018-04-17 | 上海茂涵科技有限公司 | A kind of preparation method of TiO 2 sol |
| CN107913692B (en) * | 2016-10-08 | 2020-05-26 | 瞿海锋 | Preparation method of titanium dioxide sol |
| CN107915254B (en) * | 2016-10-08 | 2020-05-26 | 瞿海锋 | Preparation method of nano titanium dioxide powder |
| CN107799756A (en) * | 2017-10-31 | 2018-03-13 | 湘潭大学 | A kind of Na2Ti3O7The preparation method of C nano fiber |
| CN107913693A (en) * | 2017-11-23 | 2018-04-17 | 中国科学院福建物质结构研究所 | The oxygen-enriched state titanium oxide in surface and preparation method for high-activity treatment of textile dye waste |
| CN110668496A (en) * | 2019-11-14 | 2020-01-10 | 大连交通大学 | Method for preparing rutile TiO by HCl volatilization low-temperature method2Nano powder |
| CN110668496B (en) * | 2019-11-14 | 2022-05-06 | 大连交通大学 | Method for preparing rutile TiO by HCl volatilization low-temperature method2Nano powder |
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| CN100424020C (en) | 2008-10-08 |
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