Fe，V共掺杂TiO_2催化剂的合成、表征及其性能研究
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摘要
本论文通过不同方法合成系列单组分掺杂、双组分共掺杂的改性纳米TiO2,探讨了不同制备条件(钛源、不同掺杂元素、掺杂比例、焙烧温度)和不同反应条件(催化剂用量、反应体系酸度、光催化)对染料脱色率的影响。采用XRD、TG-DTG、FT-IR、SEM、EDS、BET、UV-Vis DRS、XRF、TEM、XPS、ESR、ICP等现代测试手段对所制备催化剂的理化性能进行详细表征与分析。实验结果表明,以四氯化钛为钛源,通过共沉淀法制备的掺杂改性纳米Ti02具有高效的吸附性能,在接近吸附饱和后还表现出一定的可见光光催化活性。其中,共掺杂Fe-V-TiO2(Ti:Fe:V物质的量比为1：0.15：0.3,400℃焙烧2 h)具有最佳的吸附性能,60 min内对100 ppm亚甲基蓝溶液(催化剂用量为1.50g/L,反应体系酸度为中性)的脱色率可达99.01%,8h后矿化率可达89.56%；可使实际印染废水的COD由1938 mg/L降为899.56 mg/L,有效降解了废水中的污染物。表征结果表明,共掺杂的样品比表面积增大,有效拓展了Ti02在可见光范围的响应；样品在溶液中可产生较多的超氧自由基,表现出较强的氧化能力；铁物种以Fe3+的形态存在,钒物种以V5+的形态存在,且处理后溶液中钒离子浓度远小于GB 3838-2000的最高浓度,表明该类共掺杂改性催化剂具有重要的实际应用意义。
The paper probes into a series of modified nano-TiO2 via different preparation methods. The effects of different system variables like preparation conditions (sources of titanium、doping elements、doping ratioes、calcinable temperatures) and reaction conditions (different adsorbent dosage、pH value、photocatalytic activity) of catalysts are also investigated. The physicochemical properties of the catalysts are measured by XRD、TG-DTG、FT-IR、SEM、EDS、BET、UV-Vis DRS、XRF、TEM、XPS、ESR and ICP. The experimental results suggest that co-doped TiO2 synthesized via coprecipitation has an excellent ability in adsorbing, utilizing titanium tetrachloride as precursors, it also has photocatalytic activities in degradation of dye under visible light after adsorption. The Fe-V-TiO2 (the doped mole ratio of Ti:Fe:V is 1:0.15:0.3, calcined at 400℃for 2 h) exhibits the best adsorbtion activity on methylene blue (MB) solution. The decolourization rate of MB (100 ppm) surpasses 99.01% within 60 min dark reaction (the catalyst dosage is 1.50 g/L, in neutral condition). Its mineralization rate of MB rises to 89.56% within 8 h, which degrades the pollutants in wastewater effectively. The COD of actual high concentrated wastewater reduces from 1938 mg/L to 899.56 mg/L. Co-doped increases the specific surface area, and expands the response scope of TiO2 in visible light. Samples in the solutiion can produce much more O2-, which exhibits excellent oxidation ability. Fe-V-TiO2 sample can be acquired by mixing iron in Fe3+ form and vanadium in V5+ form. Such solution is of a much lower vanadium density than the maxium one in GB 3838-2000, which reveals that such a modified catalyst is of considerable significance in practical application.
The paper probes into a series of modified nano-TiO2 via different preparation methods. The effects of different system variables like preparation conditions (sources of titanium、doping elements、doping ratioes、calcinable temperatures) and reaction conditions (different adsorbent dosage、pH value、photocatalytic activity) of catalysts are also investigated. The physicochemical properties of the catalysts are measured by XRD、TG-DTG、FT-IR、SEM、EDS、BET、UV-Vis DRS、XRF、TEM、XPS、ESR and ICP. The experimental results suggest that co-doped TiO2 synthesized via coprecipitation has an excellent ability in adsorbing, utilizing titanium tetrachloride as precursors, it also has photocatalytic activities in degradation of dye under visible light after adsorption. The Fe-V-TiO2 (the doped mole ratio of Ti:Fe:V is 1:0.15:0.3, calcined at 400℃for 2 h) exhibits the best adsorbtion activity on methylene blue (MB) solution. The decolourization rate of MB (100 ppm) surpasses 99.01% within 60 min dark reaction (the catalyst dosage is 1.50 g/L, in neutral condition). Its mineralization rate of MB rises to 89.56% within 8 h, which degrades the pollutants in wastewater effectively. The COD of actual high concentrated wastewater reduces from 1938 mg/L to 899.56 mg/L. Co-doped increases the specific surface area, and expands the response scope of TiO2 in visible light. Samples in the solutiion can produce much more O2-, which exhibits excellent oxidation ability. Fe-V-TiO2 sample can be acquired by mixing iron in Fe3+ form and vanadium in V5+ form. Such solution is of a much lower vanadium density than the maxium one in GB 3838-2000, which reveals that such a modified catalyst is of considerable significance in practical application.
引文
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