CN110627116B - A hydrogen-doped TiO2 phase change nanomaterial and its application - Google Patents

A hydrogen-doped TiO2 phase change nanomaterial and its application Download PDF

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CN110627116B
CN110627116B CN201910839855.6A CN201910839855A CN110627116B CN 110627116 B CN110627116 B CN 110627116B CN 201910839855 A CN201910839855 A CN 201910839855A CN 110627116 B CN110627116 B CN 110627116B
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崔小强
贾广日
王颖
张雷
张海燕
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Abstract

本发明公开了一种氢掺杂TiO2相变纳米材料及其应用,属于清洁可持续新型能源制备应用领域。本发明主要通过调控有机强酸与水进行不同比例，在低温水热处理的情况下获得不同相氢掺杂的TiO2材料。这种掺杂增大了材料的光吸收范围，提高了对于光生载流子分离的效率，由于这两方面的原因进而大幅度提高材料的催化活性，提高了光催化产氢的催化效率，并详细的解释了这种催化效果主要来源于光吸收范围的拓宽和光生载流子的有效分离。The invention discloses a hydrogen-doped TiO2 phase-change nanomaterial and an application thereof, belonging to the field of clean and sustainable new energy preparation and application. The present invention mainly obtains TiO 2 materials with different phases of hydrogen doped under the condition of low temperature hydrothermal treatment by adjusting different ratios of organic strong acid and water. This doping increases the light absorption range of the material and improves the separation efficiency of photogenerated carriers. Due to these two reasons, the catalytic activity of the material is greatly improved, and the catalytic efficiency of photocatalytic hydrogen production is improved. It is explained in detail that this catalytic effect mainly originates from the broadening of the light absorption range and the effective separation of photogenerated carriers.

Description

Hydrogen-doped TiO (titanium dioxide)2Phase-change nano material and application thereof
Technical Field
The invention belongs to the field of clean and sustainable novel energy preparation and application, and particularly relates to hydrogen-doped TiO2Phase-change nano material and application thereof in photocatalytic hydrogen production reaction.
Background
With the continuous development of the world economy, energy and environmental problems have become one of the problems to be solved urgently. Hydrogen, a clean and renewable energy source, is gradually becoming a hot spot for the research of the majority of researchers. Compared with methods for consuming energy such as methane steam reforming, coal gasification and water electrolysis, the method for decomposing water into hydrogen by using inexhaustible natural energy, namely solar energy, is favored. Among the numerous photocatalytic materials, TiO2Due to its good chemical stability, thermal stability, environmental friendliness and suitable energy band position, it is one of the most potential photocatalytic materials and is widely used in the field of photocatalysis.
Well known TiO stabilized in existence2There are three crystal forms: anatase, rutile and brookite, but these three crystalline forms of TiO2But are not all suitable for photocatalytic water splitting. Anatase is generally better than rutile and brookite. Unfortunately, while rutile is not as characteristic as anatase, it has a better absorption range for sunlight than anatase. If the photocatalytic property of rutile is to be improved, the structure of rutile needs to be modified so as to retain the original structureUnder the condition of superiority, the light utilization rate is further widened, the recombination rate of photon-generated carriers is inhibited, and the efficiency of the photocatalyst applied to the aspect of photocatalysis is greatly promoted by solving the two problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a hydrogen-doped TiO2Phase-change nano material and is applied to the field of photocatalysis water decomposition catalysis. The hydrogen-doped TiO2The phase-change nano material has the characteristics of low price, simple preparation, high catalytic activity, good stability and the like.
The invention is realized by the following technical scheme: hydrogen-doped TiO (titanium dioxide)2Phase change nanomaterial of hydrogen doped TiO2The phase-change nano material is prepared by the following method:
(1) CF is prepared by3SO3H and water are uniformly mixed according to the volume ratio of 1: 0-1: 1 to obtain CF3SO3H aqueous solution.
(2) 4-10ml of tetrabutyl titanate is added into a polytetrafluoroethylene lined autoclave.
(3) 4ml of the CF obtained in step 1 are taken3SO3And (3) dropwise adding the H aqueous solution into the high-pressure reaction kettle in the step (2), stirring, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the high-pressure reaction kettle after uniform mixing and no precipitation, and carrying out hydrothermal treatment at the temperature of 140-.
(4) After the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed by water for 3 times, the centrifugal speed is 6000-2And (3) nano materials.
Hydrogen-doped TiO (titanium dioxide)2The application of the nano-structure material in the photocatalytic hydrogen production reaction.
Compared with the prior art, the invention has the beneficial effects that: the invention takes organic strong acid as raw material and hydrogen source, and hydrogen is introduced into TiO by the participation of hydrogen in the reaction process2In the crystal lattice and with the TiO formed2Interaction to alter TiO2Is connected withAnd (5) forming. The in-situ hydrogen-doped TiO is obtained by a simple low-temperature hydrothermal method2Compared with a hydrogen post-treatment method, the method can obtain a bulk-doped material with good crystallinity. This structure is H-doped TiO in terms of catalytic activity2The absorption range of light is widened, and the effective separation of the material on photon-generated carriers is enhanced, so that the utilization rate of the material on photocatalytic water decomposition is greatly improved.
Drawings
FIG. 1 shows hydrogen-doped TiO according to the invention2XRD pattern of phase change nano material;
FIG. 2 is a schematic representation of the present invention employing 95 vt% CF3SO3Preparation of hydrogen-doped TiO from H aqueous solution2Transmission electron microscope pictures (TEMs);
FIG. 3 is a diagram of the present invention employing 50 vt% CF3SO3Hydrogen doped TiO prepared from H aqueous solution2Transmission Electron Microscopy (TEM) of phase change nanomaterials;
FIG. 4 shows the preparation of hydrogen-doped TiO according to the present invention2Solid H nuclear magnetism of the phase-change nano material;
FIG. 5 shows hydrogen-doped TiO prepared according to the present invention2A spectral data plot of the phase change nanomaterial;
FIG. 6 shows hydrogen-doped TiO prepared according to the present invention2Phase change nanomaterials compared to the photocatalytic hydrogen production rate of commercial P25.
Detailed Description
The technical solution of the invention is further illustrated below with reference to the accompanying drawings and examples, which are not to be construed as limiting the technical solution.
Example 1
(1) CF is prepared by3SO3Mixing H and water according to the volume ratio of 1:1 to obtain CF3SO3An aqueous solution of H;
(2) adding 10ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(3) 4ml of the CF mixed in step 1 were taken out3SO3H aqueous solution is added dropwise to the high pressure reaction containing tetrabutyl titanateStirring in a kettle, then dripping 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle after uniform mixing and no precipitation, and carrying out hydrothermal treatment at 180 ℃ for 16 h;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 6000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
FIG. 1 shows the hydrogen-doped TiO prepared in this example2XRD pattern of phase-change nano material. It can be seen from the figure that 50 vt% water produces hydrogen doped TiO2Is anatase phase. FIG. 2 shows the preparation of hydrogen-doped TiO with 50 vt% water prepared in this example2Transmission Electron Microscopy (TEM) of (A) in which the anatase phase TiO prepared by this process is visible2Is nano-particle of about 10 nm. FIG. 4 shows the preparation of hydrogen-doped TiO with 50% vt water prepared in this example2Solid hydrogen nuclear magnetic field, as can be seen from the figure, this hydrogen doped TiO2The material has many forms of hydrogen. FIG. 5 shows the hydrogen-doped TiO prepared in this example2Spectral data plot of material. From the figure it can be seen that the hydrogen doped TiO with 50 vt% water2The material expands the absorption range of light.
The hydrogen-doped TiO prepared in example 1 was taken230mg of a sample is added into 80ml of 20vt percent methanol aqueous solution, 0.5wt percent platinum chloroplatinic acid solution is added into the solution (in-situ photoreduction) and is connected into a photocatalytic system (GC2014), a 300W xenon lamp is used as a light source for simulating sunlight, firstly, the sample is vacuumized for 30min, secondly, the sample is subjected to photoreduction to generate a Pt cocatalyst in situ, and then, the photocatalytic hydrogen production test is carried out.
FIG. 6 shows the hydrogen-doped TiO prepared in this example2Material versus photocatalytic hydrogen production rate of commercial P25. From the figure, it can be seen that the hydrogen-doped TiO2Compared with commercial P25, the photocatalytic hydrogen production efficiency of the material is improved by about 1.28 times under the same condition. Shows higher catalytic activity.
Example 2
(1) CF is prepared by3SO3H and water are uniformly mixed according to the volume ratio of 1:0.05 to obtain CF3SO3An aqueous solution of H;
(2) adding 10ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(3) 4ml of the CF mixed in step 1 were taken out3SO3Dropwise adding the H aqueous solution into a high-pressure reaction kettle filled with tetrabutyl titanate, stirring, after uniformly mixing and no precipitation, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle, and carrying out hydrothermal treatment at 200 ℃ for 10 hours;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 8000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
The hydrogen-doped TiO prepared in this example is shown in FIG. 12XRD pattern of phase-change nano material, from which it can be seen that 5 vt% water is used to prepare hydrogen-doped TiO2The rutile phase is rod-shaped. FIG. 3 shows the preparation of hydrogen-doped TiO with 5 vt% water prepared in this example2Transmission Electron Microscopy (TEM) of (A) from which it can be seen that the rutile phase TiO produced by this method is in the form of a powder2Is nano-particle of about 10 nm. The preparation of hydrogen doped TiO with 5% vt water prepared in this example is shown in FIG. 42Solid hydrogen Nuclear Magnetic Resonance (NMR), it can be seen from the figure that rutile phase TiO obtained by this method2The solid hydrogen nuclear magnetic spectrum (fig. 4) shows a more enhanced participation in H. The hydrogen-doped TiO prepared in this example is shown in FIG. 52Spectral data plot of material. From the figure it can be seen that the hydrogen doped TiO contains 5 vt% water2The material expands the absorption range of light.
The hydrogen-doped TiO prepared in example 2 was taken2Adding 30mg of sample into 80ml of 20 vt% methanol aqueous solution, adding 0.5 wt% platinum chloroplatinic acid solution (in-situ photoreduction) into the solution, connecting the solution into a photocatalytic system (GC2014), and using a 300W xenon lamp as a light source for simulating sunlight, firstly vacuumizing for 30min, secondly performing photoreduction to generate a Pt promoter in situ, and then performing lightAnd (5) catalytic hydrogen production test.
As can be seen from fig. 6, the photocatalytic hydrogen production efficiency of the present example is improved by about 1.74 times compared to that of commercial P25. Shows higher catalytic activity.
Example 3
(1) Adding 4ml of tetrabutyl titanate into a 50ml of high-pressure reaction kettle with a polytetrafluoroethylene lining;
(2) take out 4ml of CF3SO3Dropwise adding the H original solution into a high-pressure reaction kettle filled with tetrabutyl titanate, stirring, after uniformly mixing and no precipitation, then dropwise adding 10ml of absolute ethyl alcohol, continuously stirring, sealing the reaction kettle, and carrying out hydrothermal treatment at 140 ℃ for 16 hours;
(4) after the high-pressure reaction kettle is cooled to room temperature, the solid in the high-pressure reaction kettle in the step 3 is reserved, the solid is centrifugally washed for 3 times by water, the centrifugal condition is 8000rpm/10min, and finally the solid is dried for 8 hours in vacuum at the temperature of 80 ℃ to obtain the hydrogen-doped TiO2And (3) nano materials.
The hydrogen-doped TiO prepared in example 3 was taken230mg of a sample is added into 80ml of 20vt percent methanol aqueous solution, 0.5wt percent platinum chloroplatinic acid solution is added into the solution (in-situ photoreduction) and is connected into a photocatalytic system (GC2014), a 300W xenon lamp is used as a light source for simulating sunlight, firstly, the sample is vacuumized for 30min, secondly, the sample is subjected to photoreduction to generate a Pt cocatalyst in situ, and then, the photocatalytic hydrogen production test is carried out.
As can be seen from fig. 6, the photocatalytic hydrogen production efficiency of the present example is improved by about 1.34 times compared with that of commercial P25. Shows higher catalytic activity.

Claims (2)

1.一种氢掺杂TiO2相变纳米材料，其特征在于，所述氢掺杂TiO2相变纳米材料通过以下方法制备：1. A hydrogen-doped TiO 2 phase-change nanomaterial, characterized in that, the hydrogen-doped TiO 2 phase-change nanomaterial is prepared by the following method: （1）将CF3SO3H与水按照体积比1:0~1:1混合均匀，得到CF3SO3H溶液；(1) Mix CF 3 SO 3 H and water uniformly in a volume ratio of 1:0 to 1:1 to obtain a CF 3 SO 3 H solution; （2）将4-10 ml的钛酸四丁酯加入到聚四氟乙烯内衬的高压反应釜中；(2) Add 4-10 ml of tetrabutyl titanate to the polytetrafluoroethylene-lined autoclave; （3）取4ml步骤（1）得到的CF3SO3H溶液，逐滴加入到步骤（2）中的高压反应釜中，进行搅拌，随后滴入10ml的无水乙醇继续搅拌，待混合均匀无沉淀后，封闭高压反应釜，在140-200℃下水热处理10-16h；(3) Take 4 ml of the CF 3 SO 3 H solution obtained in step (1), add dropwise to the autoclave in step (2), stir, and then drop in 10 ml of absolute ethanol to continue stirring until the mixture is uniform After there is no precipitation, the autoclave is closed and hydrothermally treated at 140-200°C for 10-16h; （4）待高压反应釜冷却至室温后，保留步骤（3）高压反应釜中的固体，用水离心洗涤固体3次，离心速率为6000-8000rpm，离心时间为10min，最后将固体在80℃下真空干燥8小时以上，得到氢掺杂TiO2纳米材料。(4) After the autoclave is cooled to room temperature, keep the solids in the autoclave in step (3), wash the solids by centrifugation with water 3 times, the centrifugation speed is 6000-8000rpm, the centrifugation time is 10min, and finally the solids are cooled at 80°C. After vacuum drying for more than 8 hours, hydrogen-doped TiO 2 nanomaterials were obtained. 2.一种权利要求1所述氢掺杂TiO2纳米结构材料在光催化产氢反应中的应用。2 . The application of the hydrogen-doped TiO 2 nanostructure material of claim 1 in photocatalytic hydrogen production reaction. 3 .
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