CN106955683B - Visible light response TiO2Preparation method of precursor and obtained TiO2Precursor and catalyst - Google Patents

Visible light response TiO2Preparation method of precursor and obtained TiO2Precursor and catalyst Download PDF

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CN106955683B
CN106955683B CN201610017971.6A CN201610017971A CN106955683B CN 106955683 B CN106955683 B CN 106955683B CN 201610017971 A CN201610017971 A CN 201610017971A CN 106955683 B CN106955683 B CN 106955683B
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precursor
tio
visible light
catalyst
titanate
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CN106955683A (en
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赵彤
于晗
叶丽
李�昊
邱文丰
潘迅
杨自海
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Tunable Materials Co ltd
Institute of Chemistry CAS
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    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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Abstract

The invention relates to visible light responding TiO2Preparation method of precursor and obtained TiO2Precursor and catalyst, wherein the preparation method comprises the following steps: 1) putting titanate into a reaction container, adding a nitrogen-containing compound, and heating and refluxing; 2) adding a chelating agent at room temperature to 100 ℃, and heating and refluxing; 3) dripping mixed solution of water and alcohol at room temperature to 80 ℃, refluxing after dripping, reducing the temperature, and removing the solvent to obtain the TiO2And (3) precursor. The visible light responding TiO provided by the invention2The precursor can be dissolved in common solvent, so that the precursor can be loaded on fiber, sheet, porous material (such as molecular sieve) and other matrixes by simple impregnation, and then the matrix loaded with the precursor is sintered at high temperature in the air, so that the precursor is converted into visible light-responsive TiO2The photocatalyst is loaded on the substrate, which not only solves the recovery problem of the catalyst, but also solves the problem of common TiO2The catalyst has no response to visible light.

Description

Visible light response TiO2Preparation method of precursor and obtained TiO2Precursor and catalyst
Technical Field
The invention belongs to the field of material science, and particularly relates to visible light response TiO2Preparation method of precursor and obtained TiO2A precursor and a catalyst.
Background
Since the twentieth century, with the continuous development and progress of science and technology, the global industry has been unprecedented. However, the development of industry has promoted economic development and facilitated human life, but has also destroyed the environment where human lives in an inexorable manner, and the influence of air pollution and water pollution caused by the development of industry on human life has become more and more obvious. The photocatalytic oxidation technology based on semiconductor catalyst is increasingly receiving attention from scholars at home and abroad as an advanced oxidation technology. Almost all organic matters can be completely oxidized into CO under the action of photocatalysis2And H2O, and the like, and in addition, the photocatalyst can also reduce heavy metal ions in the water. Among the commonly used semiconductor photocatalysts, TiO2The photocatalyst has the advantages of high activity, good stability, no secondary pollution, no harm to human bodies, low price and the like, can mineralize various organic pollutants without selection, and becomes the photocatalyst which is most valued and has wide application prospect.
TiO2The photocatalytic property of semiconductors has been proved by many researches, but two key problems need to be solved for practical application, ① the traditional photocatalytic research is generally carried out in a suspended state photocatalytic reaction system, and TiO exists2② TiO powder is easy to agglomerate and difficult to realize continuous separation, recovery and regeneration of catalyst2The photocatalytic oxidation can be carried out only within the limited wavelength range of ultraviolet light, and the proportion of sunlight is low, so that the popularization and the application of the photocatalytic technology are limited. Thus, the catalyst is immobilized and how this is done by modifying the TiO2The property of the photocatalyst makes the photocatalyst react under visible light, and has great practical significance for the application of photocatalytic oxidation technology in air purification and water treatment.
CN102515271A discloses TiO with visible light catalytic activity2Powder and a preparation method thereof. The TiO is2The content ranges of all crystal phases of the powder are as follows: anatase (TiO)2)90-100 wt% rutile (TiO)2)0-10 wt% of the above-mentioned material, and its preparation process is characterized by using tetrabutyl titanate and anhydrousPreparing precursor solution A from ethanol and glacial acetic acid, preparing solution from redistilled water and absolute ethanol, adding hydrochloric acid to adjust pH value to 1-5, preparing dropping liquid B, dropping the dropping liquid B into the precursor solution A, stirring in water bath at constant temperature, standing for a period of time, drying, grinding and calcining to obtain TiO with high photocatalytic activity2Powder of TiO of the invention2The powder has strong light absorption and light response in a broad spectrum range, namely under the irradiation of ultraviolet light and visible light, and is TiO with visible light catalytic activity2The preparation process of the powder is simple, the equipment is low in cost, and the reaction process is easy to control, however, the invention uses two solutions, the two solutions are still powder after being mixed, the powder is dried and calcined to obtain the catalyst, but the obtained catalyst exists in a powder form, which is not beneficial to recycling of the catalyst, and even if the catalyst is recycled, the catalyst is easy to agglomerate after being recycled, so that the photocatalytic performance is reduced, and the utilization rate of titanium dioxide in unit mass is low.
"visible light active TiO2Preparation and characterization of "[ Zhao Dan, Hui Lei, et al2Preparation and characterization of [ J]The academy of Tianjin City construction, 3 months 2010, vol 16, phase 1: 33-36 with TiOSO4The nano Ti-O-N photocatalyst with visible light activity is prepared by taking ammonia water as a raw material through a chemical precipitation method, the performance of the nano Ti-O-N photocatalyst is characterized by adopting detection methods such as SEM, BET, XRD, UV-vis, ESR, XPS and the like, the catalytic activity of the photocatalyst under visible light is researched through a methyl orange solution degradation experiment, the influence of factors such as specific surface area, visible light absorption intensity, crystal structure and the like on the photocatalytic activity of the photocatalyst is discussed, the prepared nano Ti-O-N photocatalyst can strongly absorb visible light with the wavelength range of 400-plus-600 nm after heat treatment, and the visible light absorption intensity is closely related to the heat treatment temperature of powder. The photocatalysis test shows that: the photocatalyst after heat treatment at 400 ℃ has the strongest absorption to visible light, relatively larger specific surface area and more complete developed crystal structure, and therefore, the photocatalyst shows the best photocatalytic activity under the visible light. But the obtained catalyst exists in a powder form, which is not beneficial to the recycling of the catalyst,even if the titanium dioxide is recycled, the titanium dioxide is easy to agglomerate when being used for the second time after being recycled, so that the photocatalytic performance is reduced, and the utilization rate of the titanium dioxide in unit mass is low.
In summary, TiO prepared by the prior art2The photocatalyst generally exists in a powder form, the photocatalytic reaction is generally carried out in a suspended state photocatalytic reaction system, and the photocatalyst has the defects of difficult sedimentation, great recovery difficulty and TiO2The powder is easy to agglomerate, and the continuous separation, recovery, regeneration and utilization of the catalyst are difficult to realize; related research on loading of powder is also carried out, but the problems of uneven loading and easy powder falling generally exist; further, ordinary TiO2The catalyst only responds to ultraviolet light, and the ultraviolet light part in the sunlight only accounts for less than 5 percent, so the problems seriously limit TiO2The application of the photocatalyst in practice. The polymer precursor has the advantages of adjustable structure, adjustable components, convenient doping, good film forming property, easy soft template compounding and the like, and has certain advantages in the aspect of preparing supported photocatalysts, visible light responsive photocatalysts and coatings.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects and provide a visible light response TiO2A method for preparing a precursor. The precursor prepared by the preparation method provided by the invention is a high molecular organic compound, has the processing characteristic of organic high molecules, can be loaded on a fiber, a sheet or a porous material (such as a molecular sieve) and other matrixes by simple impregnation, and then the matrix loaded with the precursor is sintered at high temperature in the air, so that the precursor is inorganic and is converted into visible light-responsive TiO2The photocatalyst is loaded on the substrate, which not only solves the recovery problem of the catalyst, but also solves the problem of common TiO2The catalyst has no response to visible light.
In order to achieve the purpose, the invention adopts the following technical scheme:
visible light response TiO2The preparation method of the precursor comprises the following steps:
1) putting titanate into a reaction container, adding a nitrogen-containing compound, and heating and refluxing;
2) adding a chelating agent at room temperature to 100 ℃, and heating and refluxing;
3) dripping mixed solution of water and alcohol at room temperature to 80 ℃, refluxing after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the visible light response TiO2And (3) precursor.
In the prior art, TiO2The photocatalyst generally exists in a powder form, the photocatalytic reaction is generally carried out in a suspended state photocatalytic reaction system, and the photocatalyst has the defects of difficult sedimentation, great recovery difficulty and TiO2The powder is easy to agglomerate, and the continuous separation, recovery, regeneration and utilization of the catalyst are difficult to realize; related research on loading of powder is also carried out, but the problems of uneven loading and easy powder falling generally exist; further, ordinary TiO2The catalyst only responds to ultraviolet light, and the ultraviolet light part in the sunlight only accounts for less than 5 percent, so the problems seriously limit TiO2The application of the photocatalyst in practice.
Firstly, placing titanate into a reaction container, then adding a nitrogen-containing compound, heating and refluxing for a period of time, then adding a chelating agent at room temperature-100 ℃, heating and refluxing for a period of time, then dripping a mixed solution of water and alcohol at room temperature-80 ℃, finishing dripping and refluxing, cooling, and removing the solvent under reduced pressure to obtain the visible light response TiO2The precursor of the photocatalyst is a high molecular organic compound, has the processing characteristic of organic high molecules, can be dissolved in common solvent, can be loaded on a fiber, a sheet or a substrate of porous material (such as molecular sieve) and the like through simple impregnation, and then the substrate loaded with the precursor is sintered at high temperature in the air, so that the precursor is inorganic and is converted into TiO responding to visible light2The photocatalyst is loaded on the substrate, which not only solves the recovery problem of the catalyst, but also solves the problem of common TiO2The catalyst has no response to visible light.
In the preparation method, the molar ratio of the titanate, the nitrogen-containing compound, the chelating agent and the water is 1: (0.1-3): (0.3-1): (0.8 to 1.3).
The molar ratio of titanate, nitrogen-containing compound, chelating agent and water is not properly selected, so that a soluble precursor cannot be obtained, and precipitates can appear in the reaction process. After a large number of tests, the invention determines that the molar ratio of titanate, nitrogen-containing compound, chelating agent and water is 1: (0.1-3): (0.3-1): (0.8 to 1.3). Within this molar ratio range, a soluble precursor can be obtained.
The molar ratio of water to alcohol in the mixed solution of water and alcohol is 1: (3-20).
The heating reflux time in the step 1) is 0.5-5 h; the heating reflux time in the step 2) is 0.5-5 h; and 3) refluxing for 1-8 h.
In the step 1), the titanate is one or a mixture of more of tetraethyl titanate, tetrapropyl titanate, tetraisopropyl titanate, tetrabutyl titanate or tetraisobutyl titanate.
In the step 1), the nitrogen-containing compound is one or a mixture of more of ethanolamine, acetamide, N-dimethylacetamide, glycine or alanine, preferably ethanolamine, acetamide or N, N-dimethylacetamide.
The chelating agent in the step 2) is one or a mixture of acetylacetone and ethyl acetoacetate.
In the mixed liquid of water and alcohol in the step 3), the alcohol is one or a mixture of ethanol, normal propyl alcohol, isopropanol, normal butanol or isobutanol.
The invention also aims to provide visible light responding TiO2And (3) precursor.
The visible light-responsive TiO2The precursor is prepared by the preparation method.
The visible light-responsive TiO2The precursor is dissolved in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropyl alcohol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
The inventors responded the visible light to TiO2Precursor dissolutionAdding n-propanol, controlling the Ti content of the solution to be 2%, and adding PEG-600, wherein the mass ratio of the PEG-600 to the Ti is 1: 2, carrying out suspension coating on the prepared precursor solution on a Si sheet, and sintering at 500 ℃ for 30min to obtain the Si sheet loaded with TiO2The catalyst coating, electron micrographs of the coating taken from different angles are shown in FIGS. 1-1 and 1-2. Indicating that the visible light TiO of the invention2The precursor has good film forming property, the porosity of the film can be regulated and controlled by adding a pore-foaming agent PEG, and cracked TiO2The catalyst was well supported on Si wafers.
In the present invention, the visible light-responsive TiO is2The precursor can be dissolved in common solvent, so that the application range of the precursor is expanded, and the precursor can be used for preparing various products such as coatings, fibers and the like.
The invention also provides visible light responding TiO2A catalyst.
In particular, said TiO2The catalyst is the TiO which responds to the visible light and is prepared by the preparation method2The precursor is obtained by cracking at 350-500 ℃ in air.
Compared with the prior art, the invention has the following advantages:
in the prior art, TiO2The photocatalyst generally exists in a powder form, the photocatalytic reaction is generally carried out in a suspended photocatalytic reaction system, and TiO exists2The powder is easy to agglomerate, and the continuous separation, recovery, regeneration and utilization of the catalyst are difficult to realize; related research on loading of powder is also carried out, but the problems of uneven loading and easy powder falling generally exist; further, ordinary TiO2The catalyst only responds to ultraviolet light, and the ultraviolet light part in the sunlight only accounts for less than 5 percent, so the problems seriously limit TiO2The application of the photocatalyst in practice. The invention prepares TiO with visible light response2The photocatalyst precursor is a high molecular organic compound and has the processing characteristic of organic high molecules, so that the photocatalyst precursor can be loaded on a fiber, a sheet or a porous material (such as a molecular sieve) and other matrixes by simple impregnation, and then the matrix loaded with the precursor is burnt at high temperature in the airThe precursor is inorganized and converted into visible light-responsive TiO2The photocatalyst is loaded on the substrate, which not only solves the recovery problem of the catalyst, but also solves the problem of common TiO2The catalyst has no response to visible light. Particularly, the invention has the beneficial effect of preparing the TiO containing nitrogen in the molecular structure2The precursor has good photocatalytic capacity under ultraviolet light (under the irradiation of a 500W mercury lamp, methyl orange can be completely degraded within 25 min) and good photocatalytic capacity under visible light (under the irradiation of a 500W xenon lamp, the degradation rate of trichlorophenol is 56% in 3h, and the degradation rate of methyl orange is 52.1%).
Drawings
FIG. 1-1 shows TiO supported on Si plate2Electron microscopy of the catalyst coating;
FIG. 1-2 shows TiO supported on Si plate2Electron microscopy of the catalyst coating;
FIG. 2 is an XRD curve of the precursor treated at 450 ℃ for 3h in air.
Detailed Description
The following are specific embodiments of the present invention, which are intended to further illustrate the invention and not to limit it.
Example 1
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) putting 1mol of tetrapropyl titanate into a drying reaction kettle provided with a condensing tube and a drying tube, adding 0.1 mol of ethanolamine, and heating and refluxing for 0.5 h;
(2) adjusting the temperature to room temperature, adding 1mol of acetylacetone, and heating and refluxing for 0.5 h;
(3) adjusting the temperature to 80 ℃, dripping a mixed solution of 0.8mol of water and 2.5mol of n-propanol, refluxing for 1h after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor for 8h at 350 ℃ in air to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of methyl orange solution (the concentration is 15mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is used for illumination for 4 hours, and the degradation rate is 19.2 percent.
Example 2
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) placing 1mol of tetraisopropyl titanate in a drying reaction kettle provided with a condensing tube and a drying tube, adding 0.3mol of ethanolamine, and heating and refluxing for 1 h;
(2) adjusting the temperature to 100 ℃, adding 0.8mol of ethyl acetoacetate, and heating and refluxing for 1 h;
(3) and adjusting the temperature to room temperature, dripping a mixed solution of 1.2mol of water and 6mol of isopropanol, refluxing for 3 hours after dripping, and reducing the pressure and removing the solvent after cooling to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor at 500 ℃ for 30min to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of methyl orange solution (the concentration is 15mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is used for illumination for 4 hours, and the degradation rate is 25.7 percent.
Dissolving the precursor in n-propanol, controlling the Ti content of the solution to be 2%, and adding a pore-foaming agent PEG-600, wherein the mass ratio of PEG-600 to Ti is 1: 2, the prepared precursor solution is coated on a Si sheet in a suspension way and sintered for 30min at 500 ℃ to obtain the Si sheet loaded porous TiO2The catalyst coating, electron micrographs of the coating taken from different angles are shown in FIGS. 1-1 and 1-2, and it can be seen that the resulting coating has a porous structure. The precursor has good film forming property, the porosity of the film can be regulated and controlled by adding a pore-foaming agent PEG, and cracked TiO2The catalyst was well supported on Si wafers.
Example 3
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) putting 1mol of tetrabutyl titanate into a drying reaction kettle equipped with a condensing tube and a drying tube, adding 3mol of acetamide, and heating and refluxing for 5 hours;
(2) adjusting the temperature to room temperature, adding 0.3mol of ethyl acetoacetate, and heating and refluxing for 5 h;
(3) adjusting the temperature to 80 ℃, dripping a mixed solution of 0.8mol of water and 2.5mol of n-butyl alcohol, refluxing for 8h after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor for 3h at 450 ℃ in air to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of trichlorophenol solution (the concentration is 20mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is illuminated for 5 hours, and the degradation rate is 56 percent.
Adding 30mg of the obtained catalyst into 30ml of methyl orange solution (the concentration is 15mg/L), and illuminating for 3h by a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm), wherein the degradation rate is 52.1%, illuminating for 25min by a 500W high-pressure mercury lamp, and the degradation rate is 100%.
30mg of the obtained catalyst is added into 30ml of rhodamine B solution (the concentration is 15mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of less than 420 nm) is used for illumination for 3 hours, and the degradation rate is 26 percent. Irradiating with 500W high-pressure mercury lamp for 60min, with degradation rate of 99.6%.
The XRD curve of the precursor treated for 3h at 450 ℃ in air is shown in figure 2, and the graph shows that TiO obtained after the precursor is cracked2The catalyst is in anatase form.
Example 4
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) putting 1mol of tetraisobutyl titanate into a drying reaction kettle provided with a condensing tube and a drying tube, adding 2mol of glycine, and heating and refluxing for 2 h;
(2) adjusting the temperature to 60 ℃, adding 0.6mol of acetylacetone, and heating and refluxing for 3 h;
(3) adjusting the temperature to 40 ℃, dripping a mixed solution of 0.8mol of water and 2.5mol of n-propanol, refluxing for 5h after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor for 1h at 350 ℃ in air to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of methyl orange solution (the concentration is 20mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is used for illumination for 4 hours, and the degradation rate is 20.1 percent.
Example 5
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) placing 1mol of tetraethyl titanate in a drying reaction kettle provided with a condensing tube and a drying tube, adding 2mol of alanine, and heating and refluxing for 2 h;
(2) adjusting the temperature to 50 ℃, adding 0.6mol of acetylacetone, and heating and refluxing for 3 h;
(3) and adjusting the temperature to 75 ℃, dripping a mixed solution of 0.8mol of water and 2.4mol of isobutanol, refluxing for 5 hours after dripping, reducing the temperature, and removing the solvent to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor for 1h at 350 ℃ in air to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of methyl orange solution (the concentration is 20mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is used for illumination for 4 hours, and the degradation rate is 15%.
Example 6
Visible light responsive TiO in this example2The precursor is synthesized by the following steps:
(1) placing 1mol of tetraethyl titanate in a drying reaction kettle provided with a condensing tube and a drying tube, adding 2mol of N, N-dimethylacetamide, and heating and refluxing for 2 h;
(2) adjusting the temperature to 90 ℃, adding 0.6mol of acetylacetone, and heating and refluxing for 3 h;
(3) and adjusting the temperature to 70 ℃, dripping a mixed solution of 1.3mol of water and 26mol of ethanol, refluxing for 5 hours after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the precursor.
The precursor has better solubility in any one solvent or a mixed solvent of a plurality of solvents of ethanol, normal propyl alcohol, isopropanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, toluene or xylene.
Treating the obtained precursor for 1h at 350 ℃ in air to obtain TiO2A catalyst.
30mg of the obtained catalyst is added into 30ml of methyl orange solution (the concentration is 20mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of 420 nm) is used for illumination for 4 hours, and the degradation rate is 52.7 percent. Irradiating with 500W high-pressure mercury lamp for 30min, with degradation rate of 100%.
30mg of the obtained catalyst is added into 30ml of rhodamine B solution (the concentration is 15mg/L), a 500W xenon lamp (a filter plate filters light with the wavelength of less than 420 nm) is used for illumination for 3 hours, and the degradation rate is 36.6 percent.

Claims (8)

1. Visible light response TiO2The preparation method of the precursor is characterized by comprising the following steps:
1) putting titanate into a reaction container, adding a nitrogen-containing compound, and heating and refluxing;
2) adding a chelating agent at room temperature to 100 ℃, and heating and refluxing;
3) dripping mixed solution of water and alcohol at room temperature to 80 ℃, refluxing after dripping, reducing the temperature, and removing the solvent under reduced pressure to obtain the visible light response TiO2A precursor;
the molar ratio of the titanate, the nitrogen-containing compound, the chelating agent and the water is 1: (0.1-3): (0.3-1): (0.8 to 1.3);
the heating reflux time in the step 1) is 0.5-5 h; the heating reflux time in the step 2) is 0.5-5 h; the refluxing time in the step 3) is 1-8 h;
in the step 1), the nitrogen-containing compound is one or a mixture of more of ethanolamine, acetamide, N-dimethylacetamide, glycine or alanine.
2. The method according to claim 1, wherein the molar ratio of water to alcohol in the mixed solution of water and alcohol is 1: (3-20).
3. The method according to claim 1, wherein in step 1), the titanate is one or more selected from the group consisting of tetraethyl titanate, tetrapropyl titanate, tetraisopropyl titanate, tetrabutyl titanate, and tetraisobutyl titanate.
4. The method according to claim 1, wherein the nitrogen-containing compound is ethanolamine, acetamide or N, N-dimethylacetamide.
5. The preparation method of claim 1, wherein the chelating agent in step 2) is one or a mixture of acetylacetone and ethyl acetoacetate.
6. The method according to claim 1, wherein the alcohol in the mixture of water and alcohol in step 3) is one or more selected from ethanol, n-propanol, isopropanol, n-butanol, and isobutanol.
7. Visible light response TiO2Precursor, characterized in that it is a visible-light-responsive TiO produced by the production method according to any one of claims 1 to 62Dissolving the precursor in ethanol, n-propanol, isopropanol, and ethylene glycol monomethyl etherEthylene glycol monoethyl ether, toluene or xylene or a mixed solvent of a plurality of solvents.
8. Visible light response TiO2A catalyst, characterized in that the visible-light-responsive TiO prepared by the preparation method of any one of claims 1 to 62Cracking the precursor at 350-500 ℃ in the air to obtain the visible light response TiO2A catalyst.
CN201610017971.6A 2016-01-12 2016-01-12 Visible light response TiO2Preparation method of precursor and obtained TiO2Precursor and catalyst Active CN106955683B (en)

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