Preparation and application of organic phosphonate titanium oxide heterozygous mesoporous material
A technology of hybrid materials and mesoporous materials, which is applied in the field of preparation of porous materials, can solve problems such as the limitation of phosphonic acids, and achieve high mechanical stability, good ultraviolet and visible light catalytic performance, and high hydrothermal stability.
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Embodiment 1
[0025] Under stirring at room temperature, 1.53 g of organic phosphonic acid sodium salt EDTMPS was added to a mixed solution of 30 ml of ethanol and 15 ml of water, stirred until the solution was clear, and the pH value of the solution was adjusted to 1 with hydrochloric acid. Slowly add 1.702 g of butyl titanate dropwise, continue stirring at a slow speed for 24 hours, and crystallize at 80° C. for 24 hours. After the product is filtered, washed with water and dried, an organic / inorganic hybrid porous material (T-EDTMPS) is obtained. The samples were tested by XRD, TG-DSC, N 2 Adsorption / desorption, SEM, TEM, XPS, FT-IR, UV-vis, 31 P and 13 C MAS NMR characterization confirmed that it is an organic phosphonate titanium oxide hybrid material with mesoporous structure. Among them, TEM shows that the material has irregular worm-like mesopores ( figure 1 ); The XRD spectrum shows that the material is a single anatase crystal form ( figure 2 ); the nitrogen adsorption-desor...
Embodiment 2
[0027] Using the preparation process of Example 1, the organic phosphonic acid DTMPPA sodium salt was added to a mixed solution of 30 ml of ethanol and 15 ml of water, stirred until the solution was clear, and the pH value of the solution was adjusted to 1 with hydrochloric acid. Slowly add 1.702 g of Ti(BuOT) dropwise, continue stirring at a slow speed for 24 hours, and crystallize at 80°C for 24 hours. After the product is filtered, washed with water and dried, an organic / inorganic hybrid mesoporous material (T-DTMPPA) is obtained. Among them, TEM shows that the material has irregular worm-like mesopores ( figure 1 ); The XRD spectrum shows that the material is a single anatase crystal form ( figure 2 ); the nitrogen adsorption-desorption isotherm and the corresponding pore size distribution plots show that the material has a typical mesoporous structure ( image 3 ), the BET specific surface area is 128m 2 / g; the pore volume is 0.19cm 3 / g; the mesopore size is 3.6nm....
Embodiment 3
[0029] Get sample 0.02g in embodiment 1 and 2 and make catalyst, be suspended in the 30mg / L rhodamine B aqueous solution of 100ml, be that 125W high pressure mercury lamp and household incandescent lamp of 365nm are used as light source respectively with cut-off wavelength, Figure 4 (a) and 4(b) are comparisons of the degradation effects of samples on Rhodamine B under ultraviolet light and visible light irradiation, respectively. The second figure shows the as-synthesized hybrid material relative to the pure mesoporous TiO 2 It has high photocatalytic activity.
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