CN105110368A - Environment-friendly preparation method of pure anatase phase TiO2 with high catalytic activity under natural light - Google Patents

Environment-friendly preparation method of pure anatase phase TiO2 with high catalytic activity under natural light Download PDF

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CN105110368A
CN105110368A CN201510610728.0A CN201510610728A CN105110368A CN 105110368 A CN105110368 A CN 105110368A CN 201510610728 A CN201510610728 A CN 201510610728A CN 105110368 A CN105110368 A CN 105110368A
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environment
pure anatase
anatase tio
friendly preparation
distilled water
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CN105110368B (en
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胥焕岩
尹君垚
亓淑艳
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Harbin University of Science and Technology
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Harbin University of Science and Technology
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Abstract

The invention relates to an environment-friendly preparation method of pure anatase phase TiO2 with a high catalytic activity under natural light. The preparation method comprises the following steps: (1), weighing and taking 20-50 mL of a solvent a, a stabilizer and tetrabutyl titanate, mixing, stirring uniformly to obtain a mixed liquor A; (2), weighing and taking 5-20 mL of a solvent b and distilled water, mixing uniformly to obtain a mixed liquor B; (3), magnetic stirring while slowly and dropwise adding the mixed liquor B into the mixed liquor A until completion, stirring fully and placing the product in a reaction kettle; (4), sealing the reaction kettle, placing the sealed reaction kettle in a drying oven, heating to 130-180 DEG C, preserving heat for 3-5 h, crystallizing under the self-generated pressure, natural cooling to room temperature to obtain white turbid liquid; (5), washing the white turbid liquid with absolute ethyl alcohol and distilled water repeatedly, performing centrifugal separation until the filtrate is neutral, and drying the obtained product to obtain the pure anatase phase TiO2 polycrystalline nano-powder. The environment-friendly preparation method of the pure anatase TiO2 with a high catalytic activity under natural light can be used for preparation of TiO2.

Description

There is the pure Anatase TiO of high solar ray photocatalysis activity 2environment-friendly preparation method thereof
Technical field:
The present invention relates to a kind of pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof.Belong to surrounding purifying material and preparation field developed by photocatalyst.
Background technology:
Environmental pollution and shortage of resources are the top-priority key subjects of China the Implement of sustainable development strategy, are also the 21 century significant challenge that face of human society.Photocatalysis technology has the hydrogen manufacturing of photolysis water and the large function of photodegradation organic pollutant two, receives much attention in the field such as energy utilization, Pollution abatement.In photochemical catalysis surrounding purifying material, TiO 2have that photocatalytic activity is high, nontoxicity, stable chemical nature, do not produce secondary pollution, low cost and other advantages, be considered to the environmental friendliness shaped material of degradable organic pollutant.But, according to TiO 2band theory, TiO 2photoresponse narrow range as the weak point that photocatalyst material is maximum, TiO 2genus wide band gap semiconducter (Detitanium-ore-type, e g =3.2eV; Rutile-type, e g =3.0eV), its photocatalysis characteristic is only limited to UV light region, and UV-light only accounts for about 3 ~ 5% of sunlight, lower to the utilization ratio of sunlight.Thus, how to design better and regulate and control photocatalyst material and improve light-catalyzed reaction efficiency, effectively utilizing the object of sun power to be the focus of cut-throat competition in photocatalyst material research to reach.
2main crystalline structure has Rutile Type, Anatase and brookite, wherein Anatase TiO 2in light-catalyzed reaction process, there is higher activity and be widely studied.At present, Anatase TiO is expanded 2the means of photochemical catalysis response spectrum scope mainly comprise bulk phase-doped and surface sensitizing.The bulk phase-doped doped transition metal ions, precious metal ion doping, nonmetallic ion-doped etc. of mainly containing, surface sensitizing mainly contains precious metal ion surface sensitizing and organic dye sensitized.Although these two kinds of approach can improve Anatase TiO 2photoresponse scope, but body phase or finishing ion and dyestuff are easy to stripping in the liquid phase, while output secondary pollution, greatly reduce TiO 2the repeating utilization factor of photocatalyst, limits its applying in field of engineering technology.In addition, to Anatase TiO 2give certain form or pattern also its photoresponse scope of easily extensible, such as TiO 2nano-array, hollow bar, hollow membrane etc., but the preparation condition of these photocatalysts is very harsh, complex process, and cost is higher.In recent years, based on the Anatase TiO of first principle 2the Calculation and Study of different crystal plane surface free energy is develop visible light-responded anatase octahedrite TiO 2provide theoretical direction, preparation exposes the Anatase TiO of specific high reactivity crystal face 2become study hotspot.But, up to the present, the Anatase TiO of most exposure high reaction activity crystal faces 2preparation process in, all need to use fluorochemicals as surperficial capping agent, and fluorine-containing compound generally all has very strong toxicity or corrodibility.Therefore, adopt other preparation methods that environmental protection is nontoxic more, the Anatase TiO with high catalytic reaction activity can be prepared again at low cost simultaneously 2, be the severe challenge that photocatalysis technology field faces at present.
Summary of the invention:
The object of this invention is to provide a kind of pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof.
Above-mentioned object is realized by following technical scheme:
A kind of pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, the method comprises the steps:
(1) measure the solvent a of 20 ~ 50mL, stablizer and tetrabutyl titanate, mixing, obtains mixed liquor A after stirring;
(2) measure solvent b and the distilled water of 5 ~ 20mL, after mixing, obtain mixed liquid B;
(3), under magnetic agitation, mixed liquid B is slowly added drop-wise in mixed liquor A, after fully stir, then product is placed in reactor;
(4) sealed reactor, is placed in baking oven, and be heated to 130 ~ 180 DEG C of insulations 3 ~ 5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid;
(5) white suspension liquid dehydrated alcohol and distilled water repetitive scrubbing, centrifugation in neutral, after products therefrom oven dry, are namely obtained pure Anatase TiO to filtrate 2polycrystalline Nano powder.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, described step (1) solvent for use a is Virahol, and Virahol and tetrabutyl titanate volume ratio are 2:1 ~ 10:1, and described stablizer is Glacial acetic acid, and Glacial acetic acid and tetrabutyl titanate volume ratio are 1:1 ~ 1:5.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, the stoichiometry of amount needed for tetrabutyl titanate complete hydrolysis of described step (2) distilled water used, described solvent b is dehydrated alcohol, and the volume ratio of dehydrated alcohol and distilled water is 5:1 ~ 20:1.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, till being stirred to the appearance of light yellow clear colloidal sol after described step (3) dropwises, the packing volume of reactor is 70% ~ 80%.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, described step (4) Heating temperature is 155 DEG C, and soaking time is 4 hours.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, described step (5) drying temperature is 80 ~ 100 oC, time of drying is 30 ~ 90 minutes.
The described pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, Virahol used, Glacial acetic acid, tetrabutyl titanate and dehydrated alcohol purity are all not less than analytical pure.
Beneficial effect:
1. the present invention is on conventional hydrothermal method basis, improving technique process, screens environmental protection and general solvent and stablizer, optimizes ratio of reagents, regulation process processing parameter, prepares pure Anatase TiO undoped, have high catalytic reaction activity under natural light 2.Result of study shows, the thing phase component of obtained product only has Anatase TiO 2, be pure Anatase TiO 2polycrystalline Nano powder, under natural light, the Azo Dye-Methyl Orange of 20mg/L within 2.5 hours, can be made degradable, show high solar ray photocatalysis active.The method is simple to operate, be easy to control, with low cost, technological process environmental protection, has the realistic meaning applied.
The present invention selects solvent and the stablizer of green general-purpose, environment-protecting asepsis, has the pure Anatase TiO of high catalytic reaction activity under preparing natural light 2.The pure Anatase TiO of visible ray or natural light response is prepared compared to other 2method, the method is simple to operate, be easy to control, synthesis temperature is low, and energy consumption is few, and preparation cost is low, and agents useful for same environmental protection, nontoxic, and non-corrosiveness, has application value.
Embodiment:
Embodiment 1:
A kind of pure Anatase TiO with high solar ray photocatalysis activity 2environment-friendly preparation method thereof, the method comprises the steps:
(1) measure the solvent a of 20 ~ 50mL, stablizer and tetrabutyl titanate, mixing, obtains mixed liquor A after stirring;
(2) measure solvent b and the distilled water of 5 ~ 20mL, after mixing, obtain mixed liquid B;
(3), under magnetic agitation, mixed liquid B is slowly added drop-wise in mixed liquor A, after fully stir, then product is placed in reactor;
(4) sealed reactor, is placed in baking oven, and be heated to 130 ~ 180 DEG C of insulations 3 ~ 5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid;
(5) white suspension liquid dehydrated alcohol and distilled water repetitive scrubbing, centrifugation in neutral, after products therefrom oven dry, are namely obtained pure Anatase TiO to filtrate 2polycrystalline Nano powder.
Embodiment 2:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 2environment-friendly preparation method thereof, described step (1) solvent for use a is Virahol, and Virahol and tetrabutyl titanate volume ratio are 2:1 ~ 10:1, and described stablizer is Glacial acetic acid, and Glacial acetic acid and tetrabutyl titanate volume ratio are 1:1 ~ 1:5.
Embodiment 3:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 or 2 2environment-friendly preparation method thereof, the stoichiometry of amount needed for tetrabutyl titanate complete hydrolysis of described step (2) distilled water used, described solvent b is dehydrated alcohol, and the volume ratio of dehydrated alcohol and distilled water is 5:1 ~ 20:1.
Embodiment 4:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 or 2 or 3 2environment-friendly preparation method thereof, till being stirred to the appearance of light yellow clear colloidal sol after described step (3) dropwises, the packing volume of reactor is 70% ~ 80%.
Embodiment 5:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 or 2 or 3 or 4 2environment-friendly preparation method thereof, described step (4) Heating temperature is 155 DEG C, and soaking time is 4 hours.
Embodiment 6:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 or 2 or 3 or 4 or 5 2environment-friendly preparation method thereof, described step (5) drying temperature is 80 ~ 100 oC, time of drying is 30 ~ 90 minutes.
Embodiment 7:
The pure Anatase TiO with high solar ray photocatalysis activity according to embodiment 1 or 2 or 3 or 4 or 5 or 6 2environment-friendly preparation method thereof, Virahol used, Glacial acetic acid, tetrabutyl titanate and dehydrated alcohol purity are all not less than analytical pure.
Embodiment 8:
Accurately measure Virahol 40mL, Glacial acetic acid 2mL, butyl (tetra) titanate 10mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 1mL needed for dehydrated alcohol 10mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 3 and littlely only occur up to light yellow clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 150 oc, be incubated 4.5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 90 oCdry 30 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.
Embodiment 9:
Accurately measure Virahol 20mL, Glacial acetic acid 5mL, butyl (tetra) titanate 10mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 1mL needed for dehydrated alcohol 5mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 2 and littlely only occur up to white clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 130 oc, be incubated 4 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 90 oCdry 90 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.
Embodiment 10:
Accurately measure Virahol 50mL, Glacial acetic acid 5mL, butyl (tetra) titanate 20mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 2mL needed for dehydrated alcohol 15mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 3 and littlely only occur up to light yellow clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 180 oc, be incubated 4 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 80 oCdry 60 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.
Embodiment 11:
Accurately measure Virahol 40mL, Glacial acetic acid 10mL, butyl (tetra) titanate 20mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 2mL needed for dehydrated alcohol 10mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 3 and littlely only occur up to dark white clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 140 oc, be incubated 4.5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 100 oCdry 60 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.
Embodiment 12:
Accurately measure Virahol 30mL, Glacial acetic acid 4mL, butyl (tetra) titanate 10mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 1mL needed for dehydrated alcohol 15mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 4 and littlely only occur up to light yellow clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 160 oc, be incubated 3 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 90 oCdry 30 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.
Embodiment 13:
Accurately measure Virahol 50mL, Glacial acetic acid 10mL, butyl (tetra) titanate 10mL, mixing, stirs and obtains A liquid after 10 ~ 20 minutes; Accurately measure stoichiometric distilled water 1mL needed for dehydrated alcohol 20mL, complete hydrolysis tetrabutyl titanate, mixing, stirs and obtains B liquid after 10 ~ 20 minutes.Under magnetic agitation, mixed liquid B separating funnel is slowly added drop-wise in mixed liquor A, after fully stir 4 and littlely only occur up to light yellow clear colloidal sol, then be placed in reactor by this vitreosol, the packing volume of reactor is 70% ~ 80%.Sealed high pressure reactor, is placed in baking oven, is heated to 180 oc, be incubated 5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid.Filtered by suspension liquid, then be 7 ~ 8 with dehydrated alcohol and distilled water repetitive scrubbing, centrifugation to filtrate pH value, products therefrom is 90 oCdry 90 minutes, namely obtain pure Anatase TiO 2polycrystalline Nano powder.

Claims (7)

1. one kind has the pure Anatase TiO of high solar ray photocatalysis activity 2environment-friendly preparation method thereof, is characterized in that: the method comprises the steps:
(1) measure the solvent a of 20 ~ 50mL, stablizer and tetrabutyl titanate, mixing, obtains mixed liquor A after stirring;
(2) measure solvent b and the distilled water of 5 ~ 20mL, after mixing, obtain mixed liquid B;
(3), under magnetic agitation, mixed liquid B is slowly added drop-wise in mixed liquor A, after fully stir, then product is placed in reactor;
(4) sealed reactor, is placed in baking oven, and be heated to 130 ~ 180 DEG C of insulations 3 ~ 5 hours, crystallization at autogenous pressures, then naturally cools to room temperature, obtains white suspension liquid;
(5) white suspension liquid dehydrated alcohol and distilled water repetitive scrubbing, centrifugation in neutral, after products therefrom oven dry, are namely obtained pure Anatase TiO to filtrate 2polycrystalline Nano powder.
2. the pure Anatase TiO with high solar ray photocatalysis activity according to claim 1 2environment-friendly preparation method thereof, is characterized in that: described step (1) solvent for use a is Virahol, and Virahol and tetrabutyl titanate volume ratio are 2:1 ~ 10:1, and described stablizer is Glacial acetic acid, and Glacial acetic acid and tetrabutyl titanate volume ratio are 1:1 ~ 1:5.
3. the pure Anatase TiO with high solar ray photocatalysis activity according to claim 1 and 2 2environment-friendly preparation method thereof, is characterized in that: the stoichiometry of amount needed for tetrabutyl titanate complete hydrolysis of described step (2) distilled water used, and described solvent b is dehydrated alcohol, and the volume ratio of dehydrated alcohol and distilled water is 5:1 ~ 20:1.
4. the pure Anatase TiO with high solar ray photocatalysis activity according to claim 1 or 2 or 3 2environment-friendly preparation method thereof, is characterized in that: till being stirred to the appearance of light yellow clear colloidal sol after described step (3) dropwises, the packing volume of reactor is 70% ~ 80%.
5. the pure Anatase TiO with high solar ray photocatalysis activity according to claim 1 or 2 or 3 or 4 2environment-friendly preparation method thereof, is characterized in that: described step (4) Heating temperature is 155 DEG C, and soaking time is 4 hours.
6. the pure Anatase TiO with high solar ray photocatalysis activity according to claim 1 or 2 or 3 or 4 2environment-friendly preparation method thereof, is characterized in that: described step (5) drying temperature is 80 ~ 100 oc, time of drying is 30 ~ 90 minutes.
7. the pure Anatase TiO with high solar ray photocatalysis activity according to Claims 2 or 3 or 4 or 5 or 6 2environment-friendly preparation method thereof, is characterized in that: Virahol used, and Glacial acetic acid, tetrabutyl titanate and dehydrated alcohol purity are all not less than analytical pure.
CN201510610728.0A 2015-09-23 2015-09-23 Environment-friendly preparation method of pure anatase phase TiO2 with high catalytic activity under natural light Expired - Fee Related CN105110368B (en)

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Cited By (5)

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CN108461637A (en) * 2018-03-13 2018-08-28 常州大学 A kind of hybrid and preparation method thereof for polymer solar battery electron transfer layer
CN108461633A (en) * 2018-03-13 2018-08-28 常州大学 A kind of hybrid and preparation method thereof for perovskite solar cell electron transfer layer
CN108927126A (en) * 2018-09-06 2018-12-04 中国药科大学 A kind of visible light-responded titanium dioxide optical catalyst and preparation method thereof
CN112206757A (en) * 2020-10-13 2021-01-12 武汉理工大学 High-activity hydroxyl-rich suspensible TiO2Simple preparation method of nanocrystalline photocatalytic material
CN115433507A (en) * 2022-08-31 2022-12-06 浙江理工大学 Water-based environment-friendly coating for removing formaldehyde through photocatalysis and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103230787A (en) * 2013-04-18 2013-08-07 中国科学院长春光学精密机械与物理研究所 Preparation method of {001} surface-exposed anatase-phase titanium dioxide microsphere photocatalyst

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103230787A (en) * 2013-04-18 2013-08-07 中国科学院长春光学精密机械与物理研究所 Preparation method of {001} surface-exposed anatase-phase titanium dioxide microsphere photocatalyst

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108461637A (en) * 2018-03-13 2018-08-28 常州大学 A kind of hybrid and preparation method thereof for polymer solar battery electron transfer layer
CN108461633A (en) * 2018-03-13 2018-08-28 常州大学 A kind of hybrid and preparation method thereof for perovskite solar cell electron transfer layer
CN108927126A (en) * 2018-09-06 2018-12-04 中国药科大学 A kind of visible light-responded titanium dioxide optical catalyst and preparation method thereof
CN112206757A (en) * 2020-10-13 2021-01-12 武汉理工大学 High-activity hydroxyl-rich suspensible TiO2Simple preparation method of nanocrystalline photocatalytic material
CN112206757B (en) * 2020-10-13 2023-08-29 武汉理工大学 High-activity hydroxyl-rich suspendable TiO (titanium dioxide) 2 Simple preparation method of nanocrystalline photocatalytic material
CN115433507A (en) * 2022-08-31 2022-12-06 浙江理工大学 Water-based environment-friendly coating for removing formaldehyde through photocatalysis and preparation method thereof

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