CN-121130921-B - Preparation method and application of chlorine-containing photocatalytic material

Abstract

The invention belongs to the field of atmospheric environment purification, and discloses a preparation method and application of a chlorine-containing photocatalytic material. The preparation method comprises the following steps of (1) obtaining Nb 2 O 5 , (2) mixing and reacting Nb 2 O 5 with HCl, washing and drying to obtain an HCl-treated Nb 2 O 5 photocatalytic material Nb 2 O 5 -HCl. According to the invention, the Nb 2 O 5 is treated by HCl to construct the chlorine-containing Nb 2 O 5 composite photocatalyst, so that chlorine free radicals can be provided during photocatalytic degradation of VOCs, and the catalytic performance of the Nb 2 O 5 -based photocatalyst is further improved.

Inventors

• GUO YUNLONG
• ZHAN QIAN
• CHEN LONGWEI
• AN TAICHENG
• LI GUIYING

Assignees

• 广东工业大学

Dates

Publication Date

20260505

Application Date

20250827

Claims (5)

1. 1. The application of the chlorine-containing photocatalytic material in photocatalytic degradation of isoprene is characterized in that the illumination intensity is 2.6mW/cm 2 , and the preparation method of the chlorine-containing photocatalytic material comprises the following steps: (1) Heating, stirring and mixing a citric acid solution and a precursor of Nb to obtain a gel solid, and drying and roasting the gel solid to obtain Nb 2 O 5 ; the molar ratio of the citric acid to Nb in the Nb precursor is 4:1 to 1:4, the heating temperature is 50-120 ℃, the stirring time is 3-12 h, the roasting temperature is 300-600 ℃, the roasting atmosphere is air, and the roasting time is 2-5 h; (2) Mixing Nb 2 O 5 with HCl solution, reacting, washing, and drying to obtain an HCl-treated Nb 2 O 5 photocatalytic material Nb 2 O 5 -HCl, wherein the reaction is carried out under a sealing condition, the reaction time is 12-72 h, the photocatalytic material Nb 2 O 5 -HCl contains Nb-Cl bonds, the concentration of the HCl solution is 1.2-3 mol/L, and the mass-volume ratio of the Nb 2 O 5 to the HCl solution is 1:5-5:1 mg/mu L.
2. 2. The use according to claim 1, wherein the concentration of citric acid in the citric acid solution is 0.5-6 moL/L, and the Nb precursor is ammonium niobate oxalate or niobium pentachloride.
3. 3. The use according to claim 1, wherein in step (1) the drying temperature is 60-150 ℃ and the drying time is 6-12 h.
4. 4. The use according to claim 1, wherein in step (2) the Nb 2 O 5 is mixed with the HCl solution by immersing Nb 2 O 5 in the HCl solution.
5. 5. The use according to claim 1, wherein in step (2) the seal is removed after the reaction has ended to volatilize the HCl 12-24 h and the drying temperature is 50-70 ℃.

Description

Preparation method and application of chlorine-containing photocatalytic material Technical Field The invention belongs to the field of atmospheric environment purification, and particularly relates to a preparation method and application of a chlorine-containing photocatalytic material. Background Volatile Organic Compounds (VOCs) are generally classified into non-methane hydrocarbons, oxygen-containing organic compounds, halogenated hydrocarbons, nitrogen-containing organic compounds, sulfur-containing organic compounds, and the like, and VOCs are involved in the formation of ozone and secondary organic aerosols in the atmosphere, are important factors responsible for photochemical smog, and most VOCs have unpleasant special odors and are toxic, irritating, teratogenic, and carcinogenic. VOCs in the atmosphere are mainly from artificial sources and natural sources, wherein toluene (C 7H8) and styrene (C 8H8) are common VOCs artificial emission sources in chemical production, and isoprene (C 5H8) is a typical VOCs natural emission source. The photocatalysis technology has the remarkable advantages of mild reaction condition, no secondary pollution, low energy consumption and the like, and can utilize the redox capability of the photogenerated carriers to degrade VOCs into harmless micromolecular substances. Niobium pentoxide (Nb 2O5) is one of typical semiconductor materials, has the advantages of low toxicity, more negative conduction band edge position, good chemical stability, thermodynamic stability, high electron injection efficiency, relatively high photocatalytic activity, high recycling rate and the like, and is a good photocatalytic material, but the performance of photocatalytic degradation of VOCs of Nb 2O5 still needs to be further improved at present. Disclosure of Invention Aiming at the problems in the prior art, the invention provides a preparation method and application of a chlorine-containing photocatalytic material, and the Nb 2O5 is treated by using HCl to construct a chlorine-ion-containing Nb 2O5 composite photocatalyst, so that chlorine free radicals are provided for photocatalytic degradation of VOCs, and the catalytic performance of the Nb 2O5 -based photocatalyst is further improved. The aim of the invention is achieved by the following technical scheme: the invention provides a preparation method of a chlorine-containing photocatalytic material, which comprises the following steps: (1) Obtaining Nb 2O5; (2) Mixing the Nb 2O5 with HCl solution, reacting, washing, and drying to obtain the HCl-treated Nb 2O5 -HCl serving as the Nb 2O5 photocatalytic material. In some embodiments, in step (1), nb 2O5 is obtained by mixing a citric acid solution with a precursor of Nb under heating and stirring to obtain a gel solid, and then drying and calcining the gel solid to obtain Nb 2O5. Further, the concentration of citric acid in the citric acid solution is 0.5-6moL/L, and the Nb precursor is ammonium niobate oxalate or niobium pentachloride. Further, the molar ratio of the citric acid to Nb in the Nb precursor is 4:1 to 1:4, the heating temperature is 50-120 ℃, the stirring time is 3-12h, the drying temperature is 60-150 ℃, and the drying time is 6-12h. Further, the roasting temperature is 300-700 ℃, the roasting atmosphere is air, and the roasting time is 2-5h. In some embodiments, in step (2), the concentration of the HCl solution is 1.2-12mol/L and the mass to volume ratio of Nb 2O5 to HCl solution is 1:5 to 5:1 (mg/. Mu.L). In some embodiments, in step (2), the Nb 2O5 is mixed with the HCl solution by immersing Nb 2O5 in the HCl solution. In some embodiments, in step (2), the reaction is performed under sealed conditions for a period of time ranging from 12 to 72 hours, the seal is removed after the reaction is completed to volatilize HCl for 12 to 24 hours, and the drying temperature is 50 to 70 ℃. The invention also provides an application of the photocatalytic material prepared by the preparation method in photocatalytic degradation of VOCs. In some embodiments, the VOCs are at least one of toluene, styrene, and isoprene. Compared with the prior art, the invention has the following beneficial technical effects: (1) According to the invention, nb 2O5 is treated by using HCl, chlorine elements are introduced into the Nb 2O5, and the obtained Nb 2O5 -HCl chlorine-containing photocatalyst can activate chloride ions on the catalyst to generate chlorine free radicals under the condition of illumination, so that the photocatalytic removal efficiency of typical VOCs is improved in the catalytic degradation of the typical VOCs. (2) The chlorine-containing composite photocatalyst is prepared by adopting a gel method and a surface chlorination method, the preparation process is simple, convenient and efficient, and meanwhile, the required raw materials are rich and easy to obtain, the cost is low, and the method is suitable for large-scale industrial production. Drawings FIG. 1 is an XRD spectr