CN101318696A - Method for concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia - Google Patents
Method for concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia Download PDFInfo
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- CN101318696A CN101318696A CNA2008100649793A CN200810064979A CN101318696A CN 101318696 A CN101318696 A CN 101318696A CN A2008100649793 A CNA2008100649793 A CN A2008100649793A CN 200810064979 A CN200810064979 A CN 200810064979A CN 101318696 A CN101318696 A CN 101318696A
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Abstract
The invention relates to a method for modulating and synthesizing nano titania with high thermal stability through ammonia, which relates to a method for synthesizing the nano titania. The method solves the problem of poor thermal stability of the prior anatase titania and the problems of poor optical performance of the titania, complex technique and high cost caused by doped chemical elements in the prior method for improving the thermal stability of the anatase titania. The method comprises the following steps that: tetrabutyl titanate and anhydrous ethanol are mixed and then dripped into a mixed system which consists of the anhydrous ethanol, secondary distilled water and aquafortis, and titania sol is obtained; and the ammonia is added, mixed and poured into a reaction kettle, and a deposit obtained after hydrothermal reaction is dried, grinded and roasted, so as to obtain the nano titania with high thermal stability. The method for modulating and synthesizing the nano titania with high thermal stability through the ammonia has a simple technique and low cost; and the nano titania obtained has good thermal stability, high crystallinity and good photocatalytic property.
Description
Technical field
The present invention relates to a kind of method of synthesis of nano titanium dioxide.
Background technology
The conductor photocatalysis technology is owing to easy and simple to handle, outstanding advantages such as reaction conditions is gentle, non-secondary pollution come into one's own.In numerous semiconductor light-catalysts, titanium dioxide owing to its active height, good stability, anti-photoetch by force, characteristics such as low price and safety non-toxic enjoy favor.The photocatalytic activity of titanium dioxide mainly is subjected to the influence of size of particles, crystalline phase composition and degree of crystallinity thereof.Usually anatase titanium dioxide has higher photocatalytic activity than rutile titanium dioxide, but the anatase titanium dioxide thermostability is relatively poor, under 500～600 ℃ of relatively low temperature, be easy to just be transformed into the rutile phase, cause photocatalytic activity to descend, therefore need usually to prepare enamel coating, but influenced its use range so through high-temperature heat treatment.
At present, adopt adulterated method to improve the anatase titanium dioxide thermostability, but owing to the existence of doped element causes the poor optical properties of titanium dioxide, and required complex process, cost height.
Summary of the invention
The present invention seeks in order to solve the relatively poor and method that improves the anatase titanium dioxide thermostability of existing anatase titanium dioxide thermostability, and a kind of method of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia is provided owing to the existence of doped element causes the high problem of poor optical properties, complex process and cost of titanium dioxide.
The method of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia realizes according to the following steps: one, isopyknic tetrabutyl titanate is mixed with dehydrated alcohol and stir 20～40min, get mixed solution; Two, 20: 5: 1 by volume ratio is mixed stirring 20～40min with dehydrated alcohol, redistilled water with concentrated nitric acid, gets mixed system; Three, under stirring condition, mixed solution is added drop-wise in the mixed system, get TiO 2 sol; Four, 4: 1 by volume ratio is mixed TiO 2 sol with ammoniacal liquor, 50～70min is stirred in sealing, pour into then in the teflon-lined autoclave, hydro-thermal 5～7h postcooling is to room temperature under 150～170 ℃ condition, gained throw out drying and grinding back are warming up to 600～850 ℃ of roasting 1～3h with the temperature rise rate of 10～20 ℃/min, get the high thermal stability nano titanium oxide; Wherein the mass concentration of concentrated nitric acid is 60%～70% in the step 2; The mass concentration of ammoniacal liquor is 20%～25% in the step 4.
Add ammoniacal liquor among the present invention and improved nano titanium oxide by the transition temperature of Detitanium-ore-type to the rutile phase, transition temperature is brought up to 600～850 ℃, thereby anatase-type nanometer titanium dioxide thermostability and degree of crystallinity have been promoted, make the photocatalysis performance of anatase-type nanometer titanium dioxide good, and owing to do not introduce other element, so the good in optical property of titanium dioxide.Reaction conditions gentleness, the cost of the synthetic high thermal stability nano titanium oxide of the present invention is low, technology is simple, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the XRD spectra of gained high thermal stability nano titanium oxide in the embodiment seven.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for present embodiment concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia realizes one according to the following steps, isopyknic tetrabutyl titanate is mixed with dehydrated alcohol stir 20～40min, gets mixed solution; Two, 20: 5: 1 by volume ratio is mixed stirring 20～40min with dehydrated alcohol, redistilled water with concentrated nitric acid, gets mixed system; Three, under stirring condition, mixed solution is added drop-wise in the mixed system, get TiO 2 sol; Four, 4: 1 by volume ratio is mixed TiO 2 sol with ammoniacal liquor, 50～70min is stirred in sealing, pour into then in the teflon-lined autoclave, hydro-thermal 5～7h postcooling is to room temperature under 150～170 ℃ condition, gained throw out drying and grinding back are warming up to 600～850 ℃ of roasting 1～3h with the temperature rise rate of 10～20 ℃/min, get the high thermal stability nano titanium oxide; Wherein the mass concentration of concentrated nitric acid is 60%～70% in the step 2; The mass concentration of ammoniacal liquor is 20%～25% in the step 4.
Embodiment two: present embodiment and embodiment one are different is that the mass concentration of concentrated nitric acid in the step 2 is 65%.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that the speed that mixed solution drips in the step 3 is 20～30 droplets/minute.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that 60min is stirred in sealing in the step 4, pour into then in the teflon-lined autoclave, hydro-thermal 6h postcooling is to room temperature under 160 ℃ condition, and throw out drying and grinding back are warming up to 800 ℃ of roasting 2h with the temperature rise rate of 15 ℃/min.Other step and parameter are identical with embodiment one.
Embodiment five: present embodiment and embodiment one are different is that the mass concentration of ammoniacal liquor in the step 4 is 23%.Other step and parameter are identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is that drying is dry 7～9h under 90～100 ℃ condition in the step 4.Other step and parameter are identical with embodiment one.
Embodiment seven: the method for present embodiment concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia realizes according to the following steps: one, isopyknic tetrabutyl titanate is mixed with dehydrated alcohol and stir 30min, get mixed solution; Two, 20: 5: 1 by volume ratio is mixed stirring 30min with dehydrated alcohol, redistilled water with concentrated nitric acid, gets mixed system; Three, under stirring condition, mixed solution is added drop-wise in the mixed system, get TiO 2 sol; Four, 4: 1 by volume ratio is mixed TiO 2 sol with ammoniacal liquor, 60min is stirred in sealing, pour into then in the teflon-lined autoclave, hydro-thermal 6h postcooling is to room temperature under 160 ℃ condition, gained throw out drying and grinding back are warming up to 800 ℃ of roasting 2h with the temperature rise rate of 15 ℃/min, get the high thermal stability nano titanium oxide; Wherein the mass concentration of concentrated nitric acid is 65% in the step 2; The mass concentration of ammoniacal liquor is 23% in the step 4.
Gained high thermal stability nano titanium oxide in the present embodiment, as shown in Figure 1, thermal treatment does not see that rutile produces mutually under 800 ℃ of hot conditionss, illustrates to adopt the ammoniacal liquor modulation can improve the phase transition temperature of anatase titanium dioxide significantly, thereby improves its thermostability; As the photocatalyst for degrading rhodamine B aqueous solution, degradation rate is up to 50.8% with gained high thermal stability nano titanium oxide in the present embodiment, and it is good to illustrate through the photocatalytic activity of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia.
Claims (6)
1, a kind of method of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia, the method that it is characterized in that concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia realizes according to the following steps: one, isopyknic tetrabutyl titanate is mixed with dehydrated alcohol and stir 20～40min, get mixed solution; Two, 20: 5: 1 by volume ratio is mixed stirring 20～40min with dehydrated alcohol, redistilled water with concentrated nitric acid, gets mixed system; Three, under stirring condition, mixed solution is added drop-wise in the mixed system, get TiO 2 sol; Four, 4: 1 by volume ratio is mixed TiO 2 sol with ammoniacal liquor, 50～70min is stirred in sealing, pour into then in the teflon-lined autoclave, hydro-thermal 5～7h postcooling is to room temperature under 150～170 ℃ condition, gained throw out drying and grinding back are warming up to 600～850 ℃ of roasting 1～3h with the temperature rise rate of 10～20 ℃/min, get the high thermal stability nano titanium oxide; Wherein the mass concentration of concentrated nitric acid is 60%～70% in the step 2; The mass concentration of ammoniacal liquor is 20%～25% in the step 4.
2, the method for a kind of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia according to claim 1, the mass concentration that it is characterized in that concentrated nitric acid in the step 2 is 65%.
3, the method for a kind of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia according to claim 1 is characterized in that the speed that mixed solution drips in the step 3 is 20～30 droplets/minute.
4, the method for a kind of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia according to claim 1, it is characterized in that 60min is stirred in sealing in the step 4, pour into then in the teflon-lined autoclave, hydro-thermal 6h postcooling is to room temperature under 160 ℃ condition, and throw out drying and grinding back are warming up to 800 ℃ of roasting 2h with the temperature rise rate of 15 ℃/min.
5, the method for a kind of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia according to claim 1, the mass concentration that it is characterized in that ammoniacal liquor in the step 4 is 23%.
6, the method for a kind of concocting and synthesizing nano-titanium dioxide with high-temperature stability by using aqueous ammonia according to claim 1 is characterized in that drying is dry 7～9h under 90～100 ℃ condition in the step 4.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102216221A (en) * | 2008-11-12 | 2011-10-12 | 日产化学工业株式会社 | Titanium oxide sol manufacturing method |
| CN103480352A (en) * | 2013-09-24 | 2014-01-01 | 浙江大学 | Crystal form control method for TiO2 in TiO2-ACF photocatalysis material |
| CN103877964A (en) * | 2014-03-12 | 2014-06-25 | 浙江大学 | Preparation method of heterojunction between perovskite-phase lead titanate monocrystal nanowire and anatase-phase titanium dioxide |
| CN104353444A (en) * | 2014-11-19 | 2015-02-18 | 黑龙江大学 | Method of synthesizing metatitanic acid/TiO2 nano composite material for hydrogen production from water by photodecomposition via one-step solvothermal method |
| CN104549402A (en) * | 2014-11-04 | 2015-04-29 | 华文蔚 | Preparation method of nitrogen-and-fluorine-doped nano photosensitive visible light catalyst |
| CN110026170A (en) * | 2019-05-23 | 2019-07-19 | 乐山师范学院 | A kind of TiO of photocatalytic degradation rhodamine B2Photochemical catalyst and preparation method thereof |
| CN112678867A (en) * | 2020-12-25 | 2021-04-20 | 苏州锦艺新材料科技有限公司 | Rutile type titanium dioxide and preparation method and application thereof |
| CN113398910A (en) * | 2021-05-21 | 2021-09-17 | 魏富春 | Antibacterial wastewater treatment agent and preparation method thereof |
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2008
- 2008-07-23 CN CNA2008100649793A patent/CN101318696A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102216221B (en) * | 2008-11-12 | 2014-09-10 | 日产化学工业株式会社 | Titanium oxide sol manufacturing method |
| CN102216221A (en) * | 2008-11-12 | 2011-10-12 | 日产化学工业株式会社 | Titanium oxide sol manufacturing method |
| CN103480352B (en) * | 2013-09-24 | 2015-08-12 | 浙江大学 | TiO 2tiO in-ACF catalysis material 2crystal formation control method |
| CN103480352A (en) * | 2013-09-24 | 2014-01-01 | 浙江大学 | Crystal form control method for TiO2 in TiO2-ACF photocatalysis material |
| CN103877964A (en) * | 2014-03-12 | 2014-06-25 | 浙江大学 | Preparation method of heterojunction between perovskite-phase lead titanate monocrystal nanowire and anatase-phase titanium dioxide |
| CN103877964B (en) * | 2014-03-12 | 2016-09-14 | 浙江大学 | A kind of preparation method of the hetero-junctions of Perovskite Phase lead titanate monocrystal nano line and anatase phase titanium dioxide |
| CN104549402A (en) * | 2014-11-04 | 2015-04-29 | 华文蔚 | Preparation method of nitrogen-and-fluorine-doped nano photosensitive visible light catalyst |
| CN104353444A (en) * | 2014-11-19 | 2015-02-18 | 黑龙江大学 | Method of synthesizing metatitanic acid/TiO2 nano composite material for hydrogen production from water by photodecomposition via one-step solvothermal method |
| CN110026170A (en) * | 2019-05-23 | 2019-07-19 | 乐山师范学院 | A kind of TiO of photocatalytic degradation rhodamine B2Photochemical catalyst and preparation method thereof |
| CN110026170B (en) * | 2019-05-23 | 2022-07-08 | 乐山师范学院 | TiO for degrading rhodamine B through photocatalysis2Photocatalyst and preparation method thereof |
| CN112678867A (en) * | 2020-12-25 | 2021-04-20 | 苏州锦艺新材料科技有限公司 | Rutile type titanium dioxide and preparation method and application thereof |
| CN112678867B (en) * | 2020-12-25 | 2022-01-14 | 苏州锦艺新材料科技股份有限公司 | Rutile type titanium dioxide and preparation method and application thereof |
| CN113398910A (en) * | 2021-05-21 | 2021-09-17 | 魏富春 | Antibacterial wastewater treatment agent and preparation method thereof |
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