CN107986380B - N-doped wrapped TiO2Process for degrading wastewater by using photocatalyst - Google Patents
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Abstract
The invention discloses a treatment process for photocatalytic degradation of dye wastewater, wherein a visible light catalyst adopted by the treatment process is N-doped disordered nano-encapsulated TiO2A photocatalyst. The catalyst is used for preparing disordered nano-encapsulated TiO with a thin multi-layer core-shell structure2Then, N is doped in situ in the crystal lattice, and the specificity of the structure and the doping of N elements jointly improve the TiO2Photocatalytic degradation activity on organic dyes. The invention solves the problem of low degradation efficiency of dye wastewater in the prior art, and is suitable for degrading organic dye in polluted water.
Description
Technical Field
The invention relates to a treatment process for photocatalytic degradation of dye wastewater, which adopts N-doped disordered nano-encapsulated TiO2Photocatalyst, special structure of the photocatalyst and N element in TiO2The doping among crystal lattices obviously improves TiO2The visible light catalytic activity of the photocatalyst, and the treatment process has the advantages of simple operation, low cost, high degradation efficiency and the like.
Background
In the process of textile printing and dyeing, a large amount of assistants which pollute the environment and are harmful to human bodies are used, and most of the assistants are discharged in a liquid form and inevitably enter a water body environment to cause water body pollution. For example, rhodamine B dye has carcinogenicity and mutagenicity, and rhodamine B-containing wastewater has deep chromaticity, high organic pollutant content and poor biodegradability, and is difficult to treat by conventional methods such as physical adsorption method, Fenton method and the like, so that the polluted water quality deteriorates for a long time, and the water environment and human health are seriously harmed, therefore, the degradation treatment of the wastewater is very important and urgent.
However, how to use clean energy efficiently and at low cost is still a great challenge and has profound significance. Therefore, people urgently need to develop and utilize new energy sources with environmental protection and high energy storage capacity, such as solar energy, wind energy, tidal energy, biological energy, hydrogen energy, ocean energy and the like, can economically and effectively replace fossil and mineral resources, and realize effective conversion of the energy sources without influencing normal life of people on the premise of protecting the environment and human health. In recent years, a large number of novel environment-friendly materials are produced at the same time. Nano TiO 22The material is the green functional material which can purify the environment and efficiently utilize the solar energy. It not only has oxidationThe photocatalyst has the advantages of strong capacity, excellent chemical stability, energy consumption, no subsequent secondary pollution and the like, and has the characteristics of low price, no toxicity, no harm, long-term use and the like, so the photocatalyst is favored and paid attention to by photocatalytic scientific research workers in recent years, and is widely applied to the new energy fields such as dye-sensitized solar cells, photolysis water hydrogen production, microwave adsorption, light adsorption, biological medicine treatment, photovoltaic cells, photocatalysis, lithium ion batteries and the like.
But semi-conducting TiO2The materials also have some serious disadvantages, such as pure TiO2The photocatalyst has short life of photo-generated electron-hole pairs, narrow light absorption range and low light conversion efficiency, and limits the application of the solid powder catalyst. Therefore, the morphology of the nano titanium dioxide needs to be modified and researched, and the improvement of the sunlight absorption efficiency of the nano titanium dioxide is urgent. Therefore, more and more attention is paid to the rational utilization of solar energy and semiconductor oxide to prepare hydrogen energy and effectively control the environment.
The discovery of TiO of solar photovoltaic cells under ultraviolet irradiation by Japanese scientists Fujishima and Honda since 19722Since the interesting phenomenon of water photolysis occurs in the electrode, researchers invest a great deal of effort to research TiO nearly half a century2The modification, exposition and analysis of the catalytic mechanism of the compound are carried out, and with the continuous and deep research, the photocatalytic reaction mechanism is more clear and clearer, and the modification relates to TiO2The research of (1) is focused quickly, and various progress is made in various aspects, but the research is still in the theoretical research stage of a laboratory on the whole, and has a great distance from the industrial application, so as to effectively improve the TiO2The catalytic activity of the catalyst is improved by changing the internal crystal structure and the external surface composition and property of the catalyst by the methods of compounding a narrow-band-gap semiconductor with the narrow-band-gap semiconductor, doping metal non-metal ions, depositing noble metal, photosensitizing the surface and the like, so that the band gap distance of the catalyst is reduced, the absorption capacity of the catalyst on visible light is improved, and the TiO is enhanced2The purpose of the photocatalytic performance.
In recent years, Mao et al adopted a breakthrough hydrogenation method to prepareA disordered nano TiO2TiO prepared by the method2The energy gap of the photocatalyst is only 1.54eV, and the photocatalyst has excellent visible light absorption performance and hydrogen production performance by water photolysis, but the photocatalyst is modified by doping, and the photocatalyst is used for degrading organic pollutants in water and related degradation processes, so that no systematic research is carried out.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a treatment process for degrading dye wastewater through photocatalysis, wherein the dye in the wastewater is degraded in a photocatalysis way, and the adopted photocatalyst is N-doped disordered nano-encapsulated TiO2。
The technical scheme for realizing the invention is as follows: adopts a visible light degradation mode to treat dye wastewater and prepares an N-doped disordered nano-coated TiO with excellent photocatalytic degradation activity2A photocatalyst.
The treatment process for the visible light degradation dye wastewater comprises the following steps:
coating disordered nanometer TiO doped with N2Adding a photocatalyst into dye wastewater with the concentration of 8-25 mg/L, and carrying out normal-temperature stirring visible light catalytic reaction for 0.5-3 h under a 400-600W xenon lamp, wherein the ratio of the photocatalyst to the dye wastewater is 35-45 g: and (3) 100L, wherein the distance between a xenon lamp and the liquid surface of the dye wastewater is 18-22 cm, and after the light reaction is carried out for a period of time, the xenon lamp is turned off to finish the degradation of the dye. The dye is at least one of methyl orange, methylene blue and rhodamine B.
The N-doped disordered nano-encapsulated TiO2The preparation method comprises the following steps:
disordered nano coated TiO2The preparation of (1):
a. adding TiO into the mixture2And NaBH4Mixing and grinding for 0.5-1 h to obtain a mixture, wherein the TiO is2With NaBH4The mass ratio of (1): (0.6-0.7);
b. b, transferring the mixture obtained in the step a into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 300-400 ℃ at the speed of 10-20 ℃/min under the nitrogen atmosphere, maintaining the temperature for 0.5-1 h under the condition, and then cooling the mixture to room temperature along with the furnace to obtain reacted powder;
c. b, transferring the powder obtained in the step b into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the alumina crucible to 300-400 ℃ from room temperature at a speed of 10-20 ℃/min under the argon atmosphere, maintaining the temperature for 0.5-1 h under the condition, then cooling the alumina crucible to room temperature along with the furnace, washing the alumina crucible with ethanol and water for multiple times, and drying the alumina crucible to obtain reacted powder;
d. c, mixing the powder obtained in the step c with NaBH again4Mixing, grinding for 1-2 h to obtain a mixture, mixing the powder obtained in the step c with NaBH4The mass ratio of (1): (0.8 to 0.9);
e. transferring the mixture obtained in the step d into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 300-400 ℃ at the speed of 2-5 ℃/min under the argon atmosphere, maintaining the temperature for 0.5-1 h under the condition, and then cooling the mixture along with the furnace to obtain reacted powder;
f. washing the reacted powder with ethanol and deionized water for 2-5 times respectively, and finally drying in a blast drying oven to obtain TiO2Powder;
g. the TiO obtained in the step f2Transferring the powder into an alumina crucible, placing the alumina crucible into a tubular furnace, heating the alumina crucible from room temperature to 300-500 ℃ at the speed of 2-5 ℃/min in the air atmosphere, treating the alumina crucible for 0.5-2 h under the condition, and cooling the alumina crucible to room temperature along with the furnace to obtain disordered nano-coated TiO2。
The disordered nano-encapsulated TiO2Has a multilayer core-shell structure of TiO in sequence from inside to outside2The thin multilayer core-shell structure enhances the rapid conduction of photogenerated electrons and the separation of the photogenerated electrons from holes.
II, N doped disordered nano wrapped TiO2The preparation of (1):
coating a certain amount of disordered nano prepared in the step oneTiO2Mixing with urea uniformly, placing in a tube furnace filled with inert atmosphere, heating from room temperature to 400-500 ℃ at the speed of 2-5 ℃/min, maintaining for 2h, and cooling to room temperature along with the furnace to obtain the N-doped disordered nano-coated TiO2Wherein the disordered nano-encapsulated TiO2The mass ratio of the urea to the urea is 1: (0.3-0.5).
Rhodamine B (RhB), also commonly called safflower powder, has a maximum absorption wavelength of 553.2 nmn. The rhodamine B dye is originally used as an organic xanthene dye, has certain toxicity, has strong absorbance in aqueous solution, is less influenced by external conditions, and is simple and convenient in test process, so that RhB is selected as a target pollutant to simulate and evaluate the catalytic efficiency of the catalytic material.
The specific test method is as follows: 100mL of 10mg/L RhB solution is prepared to be used as a reaction pollutant, and a proper amount of N-doped disordered nano-coated TiO is added2And putting the mixture into an ultrasonic cleaner for ultrasonic dispersion for a certain time. Then, the solution was placed in a dark box, and the degradation activity of the catalyst was examined at different times under irradiation with a xenon lamp or the like which had been used for filtering out ultraviolet light.
Compared with the prior art, the invention has the following advantages:
1. compared with the prior art, the treatment method has the advantages of simple operation, easy control of reaction conditions, low cost and potential industrial application prospect;
2. the preparation reaction condition of the photocatalyst is mild, the operation is simple, and the danger is small. TiO with multilayer core-shell structure is prepared by simple annealing step2TiO of this special multilayer core-shell structure2The photocatalyst more effectively inhibits the recombination of photoproduction electrons and holes, prolongs the service life of the electrons and the holes, increases the electron concentration and obviously improves the activity when the photocatalyst is used for degrading dyes;
3. doping of N enables the N element to enter TiO2In the crystal lattice of (2), the N element raises TiO to cause crystal lattice distortion2Specific surface area of catalyst capable of improving visible light transmittance of catalystAbsorption capacity, thereby improving the visible light catalytic efficiency of the material.
Detailed Description
The invention will now be further illustrated by reference to specific examples.
Example 1
Disordered nano coated TiO2The preparation of (1):
a. adding TiO into the mixture2And NaBH4Mixing and grinding for 0.5h to obtain a mixture, wherein the TiO is2With NaBH4The mass ratio of (1): 0.65;
b. b, transferring the mixture obtained in the step a into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 350 ℃ at the speed of 10 ℃/min under the nitrogen atmosphere, maintaining the temperature for 0.5h under the condition, and then cooling the mixture to room temperature along with the furnace to obtain reacted powder;
c. b, transferring the powder obtained in the step b into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the alumina crucible from room temperature to 400 ℃ at the speed of 10 ℃/min under the argon atmosphere, maintaining the temperature for 0.5h under the condition, then cooling the alumina crucible to room temperature along with the furnace, washing the alumina crucible with ethanol and water for multiple times, and drying the alumina crucible to obtain reacted powder A;
d. c, mixing the powder A obtained in the step c with NaBH again4Mixing and grinding for 1.5h to obtain a mixture, wherein the powder A obtained in the step c is mixed with NaBH4The mass ratio of (1): 0.85;
e. transferring the mixture obtained in the step d into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 400 ℃ at the speed of 2 ℃/min under the argon atmosphere, maintaining the temperature for 0.5h under the condition, and then cooling the mixture along with the furnace to obtain reacted powder;
f. washing the reacted powder with ethanol and deionized water for 2-5 times respectively, and finally drying in a blast drying oven to obtain TiO2Powder;
g. the TiO obtained in the step f2Transferring the powder into an alumina crucible, placing the alumina crucible into a tubular furnace, heating the alumina crucible from room temperature to 300-500 ℃ at the speed of 2-5 ℃/min in the air atmosphere, treating the alumina crucible for 0.5-2 h under the condition, and cooling the alumina crucible to the room temperature along with the furnaceWarm to obtain disordered nano-encapsulated TiO2And (3) powder B.
II, N doped disordered nano wrapped TiO2The preparation of (1):
a certain amount of disordered nano coated TiO prepared in the step one2Uniformly mixing the powder B and urea, placing the mixture in a tubular furnace filled with inert atmosphere, heating the mixture from room temperature to 400 ℃ at the speed of 2 ℃/min, maintaining the temperature for 2 hours, and then cooling the mixture to room temperature along with the furnace to obtain the N-doped disordered nano-coated TiO2Wherein the powder A or the disordered nano-encapsulated TiO2The mass ratio of the urea to the urea is 1: (0.3-0.5).
The treatment process of the RhB wastewater comprises the following steps: preparing three portions of 10mg/L RhB solution 100mL serving as reaction pollutants, and respectively adding the undoped powder A, the undoped powder B and the N-doped disordered nano-encapsulated TiO which are prepared in the same amount as in example 12And putting the mixture into an ultrasonic cleaner for ultrasonic dispersion for 0.5 h. Then putting the solution into a dark box for 30min, keeping the liquid level distance between a xenon lamp and dye wastewater at 20cm, and then sampling and analyzing the concentration of RhB in the sample liquid every 30min under the irradiation of the xenon lamp for filtering ultraviolet light, thereby inspecting the degradation activity of the catalyst at different times, wherein the specific data is shown in the following table 1:
TABLE 1 photocatalytic activity testing of different samples
As is clear from the data analysis in Table 1, it is found that the disordered nano-encapsulated TiO subjected to the reduction and oxidation treatment twice is more preferable than the powder A subjected to the reduction and oxidation treatment once2The activity of photocatalytic degradation of RhB is obviously stronger, because the multi-layer core-shell structure which is gradually thinned from inside to outside and introduced after two times of treatment enhances the rapid conduction of photoproduction electrons and the separation of the photoproduction electrons from holes, thereby enhancing TiO2Photocatalytic activity of (1). In addition, as can also be seen from the above table, the doping of the N element can also significantly improve the disordered nano-encapsulated TiO2Photocatalytic activity of (1). It can be seen that the scheme of the present invention produces N dopingDisordered nano-encapsulated TiO of2Has excellent photocatalyst degrading effect.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (1)
1. A treatment process for degrading dye wastewater by visible light comprises the following steps:
coating disordered nanometer TiO doped with N2Adding a photocatalyst into dye wastewater with the concentration of 8-25 mg/L, and carrying out normal-temperature stirring visible light catalytic reaction for 0.5-3 h under a 400-600W xenon lamp, wherein the ratio of the photocatalyst to the dye wastewater is 35-45 g: the distance between a xenon lamp and the liquid level of the dye wastewater is 18-22 cm, and after the light reaction is carried out for a period of time, the xenon lamp is turned off to complete the degradation of the dye;
the dye is at least one of methyl orange, methylene blue and rhodamine B;
the N-doped disordered nano-encapsulated TiO2The preparation method of the visible light catalyst comprises the steps of firstly preparing disordered nano-encapsulated TiO with a thin multi-layer core-shell structure2Then on TiO2Doping N element into crystal lattice;
the disordered nano-encapsulated TiO of the thin multilayer core-shell structure2The preparation method comprises the following steps:
a. adding TiO into the mixture2And NaBH4Mixing and grinding for 0.5-1 h to obtain a mixture, wherein the TiO is2With NaBH4The mass ratio of (1): (0.6-0.7);
b. b, transferring the mixture obtained in the step a into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 300-400 ℃ at the speed of 10-20 ℃/min under the nitrogen atmosphere, maintaining the temperature for 0.5-1 h under the condition, and then cooling the mixture to room temperature along with the furnace to obtain reacted powder;
c. b, transferring the powder obtained in the step b into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the alumina crucible to 300-400 ℃ from room temperature at a speed of 10-20 ℃/min under the argon atmosphere, maintaining the temperature for 0.5-1 h under the condition, then cooling the alumina crucible to room temperature along with the furnace, washing the alumina crucible with ethanol and water for multiple times, and drying the alumina crucible to obtain reacted powder;
d. c, mixing the powder obtained in the step c with NaBH again4Mixing, grinding for 1-2 h to obtain a mixture, mixing the powder obtained in the step c with NaBH4The mass ratio of (1): (0.8 to 0.9);
e. transferring the mixture obtained in the step d into an alumina crucible, then placing the alumina crucible into a tubular furnace, heating the mixture from room temperature to 300-400 ℃ at the speed of 2-5 ℃/min under the argon atmosphere, maintaining the temperature for 0.5-1 h under the condition, and then cooling the mixture along with the furnace to obtain reacted powder;
f. washing the reacted powder with ethanol and deionized water for 2-5 times respectively, and finally drying in a blast drying oven to obtain TiO2Powder;
g. the TiO obtained in the step f2Transferring the powder into an alumina crucible, placing the alumina crucible into a tubular furnace, heating the alumina crucible from room temperature to 300-500 ℃ at the speed of 2-5 ℃/min in the air atmosphere, treating the alumina crucible for 0.5-2 h under the condition, and cooling the alumina crucible to room temperature along with the furnace to obtain disordered nano-coated TiO2；
Said at TiO2The method for doping N element in crystal lattice is as follows: a certain amount of prepared disordered nano-encapsulated TiO2Mixing with urea uniformly, placing in a tube furnace filled with inert atmosphere, heating from room temperature to 400-500 ℃ at the speed of 2-5 ℃/min, maintaining for 2h, and cooling to room temperature along with the furnace to obtain the N-doped disordered nano-coated TiO2Wherein the disordered nano-encapsulated TiO2The mass ratio of the urea to the urea is 1: (0.3-0.5).
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| CN108607597A (en) * | 2018-05-24 | 2018-10-02 | 青岛理工大学 | Method for photocatalytic reduction of Cr (VI) under visible light |
| CN110280284B (en) * | 2019-06-09 | 2022-03-25 | 浙江理工大学 | A method for the simultaneous preparation of C3N4 and TiOxN2-x visible light catalysts |
| CN112117020B (en) * | 2020-09-09 | 2022-11-22 | 中国工程物理研究院核物理与化学研究所 | Method for treating tritium water by photo-thermal concerted catalysis |
| CN114247458B (en) * | 2020-09-23 | 2024-02-13 | 国家能源投资集团有限责任公司 | Preparation method and application of nitrogen-doped titanium dioxide denitrification catalyst |
| CN117483010A (en) * | 2024-01-03 | 2024-02-02 | 山东海化集团有限公司 | Modified nano TiO 2 Preparation method and application of catalyst |
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