炭吸附材料负载掺杂纳米TiO_2的制备及其降解有机污染物的研究
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摘要
本文通过对纳米TiO_2进行掺杂改性，选用比表面积高的炭材料，研究活性炭、活性炭纤维负载TiO_2的制备条件与催化降解性能的影响，为纳米TiO_2光催化、光电催化降解有机污染物技术进一步实用化提供理论依据。
在用Ti(SO_4)_2沉淀法制备的TiO_2前驱物中掺杂不同浓度的柠檬酸铁及同一浓度下不同阴离子的铁盐，并增加超声波(80℃水浴)干燥过程，经煅烧后获得高光催化活性的纳米TiO_2粉末。光催化实验结果表明，在紫外灯(主波长365nm)及太阳光下，当掺柠檬酸铁时，最佳Fe~(3+)掺杂量为0.05％摩尔比，光催化活性超过Degussa P25；当Fe~(3+)掺杂量超过1％时，显示低的光催化活性，虽然在350-500nm的波长范围有强烈的吸收和吸收边红移。当采用不同无机阴离子铁盐掺杂时，对纳米TiO_2的光催化性能影响程度与阴离子的极化力有关，带入的SO_4~(2-)使光催化性能提高最大。
采用正交试验设计方法通过浸渍法并超声分散制备出炭材料负载纳米TiO_2(TiO_2／C)催化剂，探讨了TiO_2／C催化剂制备条件，研究了该种催化剂对甲基橙溶液光／光电催化降解效果的影响，发现负载物的比表面积对于催化剂的降解率起决定性作用。通过正交实验设计方法制备多元素离子掺杂的TiO_2／活性炭(TiO_2／AC)催化剂，实验结果表明，B~(3+)的加入量对TiO_2／GAC降解甲基橙的影响最大，H_2SO_4、Fe~(3+)的影响次之，所制备样品的光催化和光电催化降解速率符合Langmurir-Hinshelwoood的假一级动力学方程，吸附为控制步骤。
通过溶胶—凝胶方法制备的颗粒活性炭(GAC)负载型的催化剂TiO_2／GAC，并以亚甲基蓝染料降解反应为模型反应，在室温和施加电压的条件下，研究了不同负载比例对活性炭原位吸附再生的关系；并且探讨了分别填充TiO_2/GAC及GAC在固定床实验装置中通入自来水进行TOC去除实验的差异。实验表明，负载TiO_2的活性炭提高了电催化再生吸附能力，负载量越高多次再生能力越强，从而降低经处理自来水中TOC的效果也越明显。
采用浸渍法在不同活性炭纤维材料(AFC)及泡沫镍上负载TiO_2，并以正交实验采用TiO_2在不同负载材料、层数、煅烧温度、硫酸、Fe~(3+)的加入量下制备吸附型光催化剂，用动态测试法研究各因数对苯的光催化降解率的影响。结果表明，TiO_2催化剂负载在ACF上，在一定质量浓度的TiO_2前驱溶胶中浸涂两层，250℃下煅烧一小时，加入适量的硫酸条件下对苯具有良好的降解性能；本研究中，最佳的掺杂铁离子量是0.10％。所制备样品的光催化降解苯的速率也符合Langmurir-Hinshelwoood的假一级动力学方程，吸附为控制步骤。
In the current work, the influence on preparing condition using the different large surface area material as supports, such as granular actived carbons and actived carbon fibers to the photocatalytic degradation performance activity have been investigated. Some new progresses were expected in the practical applications of photocatalytic technology.
Fe~(3+) doped nanometer TiO_2 photocatalysts was prepared with different content ferric citrate and different opposite anions of Fe using the Ti(SO_4)_2 precipitation method. the precursor of TiO_2 was dried over steam bath at 80℃with ultrasonic wave, then was calcined to form the high photocatalytic activities of nanometer Fe~(3+) doped TiO_2. The photocatalyst acitivity results indicated that the optimum doping amount of iron ion when doping ferric citrate was 0.05 mole% under UV and solar light and the photocatlytic activity even higher than that of Degussa P25 TiO_2,Over 1% Fe content doped TiO_2 powders showed a strong absorption in whole range 350-500 nm and a red shift in the band gap but showed the weaker photocatalytic activity. SO_4~(2-) ion doping can improve the photocatalytic degradation of TiO_2 and have better activity than that of doped with other different kind inorganic anions of Fe~(3+) salt.
The photocatalyst acitivity of nanometer titanium dioxide/ carbon material (TiO_2/C) was prepared by dip-coating technique by means of orthogonal experimental method. The effects of the conditions of prepared TiO_2/C catalyst on the photoelectrocatalysis degradation of methyl orange solution was investigated. The result was obtained that the specific surface areas of supporter play a decisive role in the degradation efficiency of methyl orange. The nano-sized TiO_2 was supported on active carbon (AC) were prepared by means of orthogonal experimental method too. The result showed that main influencing factor of photocatalysis activity was the doping amount of B~(3+) and H_2SO_4, and the effect of Fe~(3+) was much less. The kinetics of this degradation reaction conform to the Langmiur-Hinshelwood pseudo-first order kinetics model very well, and the absorption of OM on the prepared catalyst surface was the controlling step in the whole degradation process.
The adsorption and regeneration characteristics of TiO_2 supported on granular activated carbon were studied by using the electrical catalytic degradation, using methylene blue as a model organic pollutant. At the room temperature and electric voltage of 80V, the relation between removal efficiency and the loaded mass of TiO_2 was measured. The TOC removal in tap water was also used to test the efficiency packed both TiO_2/GAC and GAC into a packed-bed reactor as an adsorbent and catalyst in the electrochemical reaction. The experimental results show that loaded TiO_2 on GAC enhanced the electrical catalytic adsorption and regeneration capacity. That is, the more mass was loaded, the better regenerating performance was got, and the best TOC removal was obtained when ratio of TiO_2 to GAC was 0.8:1.
The TiO_2 photocatalyst were prepared by using dip-coating technique adhered precursor of TiO_2 to active carbon fiber and porous nickel mesh. The effects of different prepared factors, such as different supported materials, the times of coating, the calcining temperature and the added amount of H_2SO_4 were studied in photocatalytic oxidation of Benzene. The result showed that the ACF loaded with precursor of TiO_2 should be coated two times, calcined for 1 hours at 250℃and added proper amount of H2SO4. In this study, the optimum Fe~(3+) doping amount was ontained at 0.10%. And the kinetics of this degradation reaction of Benzene also corform to the Langmiur-Hinshelwood pseudo-first order kinetics model very well.
在用Ti(SO_4)_2沉淀法制备的TiO_2前驱物中掺杂不同浓度的柠檬酸铁及同一浓度下不同阴离子的铁盐，并增加超声波(80℃水浴)干燥过程，经煅烧后获得高光催化活性的纳米TiO_2粉末。光催化实验结果表明，在紫外灯(主波长365nm)及太阳光下，当掺柠檬酸铁时，最佳Fe~(3+)掺杂量为0.05％摩尔比，光催化活性超过Degussa P25；当Fe~(3+)掺杂量超过1％时，显示低的光催化活性，虽然在350-500nm的波长范围有强烈的吸收和吸收边红移。当采用不同无机阴离子铁盐掺杂时，对纳米TiO_2的光催化性能影响程度与阴离子的极化力有关，带入的SO_4~(2-)使光催化性能提高最大。
采用正交试验设计方法通过浸渍法并超声分散制备出炭材料负载纳米TiO_2(TiO_2／C)催化剂，探讨了TiO_2／C催化剂制备条件，研究了该种催化剂对甲基橙溶液光／光电催化降解效果的影响，发现负载物的比表面积对于催化剂的降解率起决定性作用。通过正交实验设计方法制备多元素离子掺杂的TiO_2／活性炭(TiO_2／AC)催化剂，实验结果表明，B~(3+)的加入量对TiO_2／GAC降解甲基橙的影响最大，H_2SO_4、Fe~(3+)的影响次之，所制备样品的光催化和光电催化降解速率符合Langmurir-Hinshelwoood的假一级动力学方程，吸附为控制步骤。
通过溶胶—凝胶方法制备的颗粒活性炭(GAC)负载型的催化剂TiO_2／GAC，并以亚甲基蓝染料降解反应为模型反应，在室温和施加电压的条件下，研究了不同负载比例对活性炭原位吸附再生的关系；并且探讨了分别填充TiO_2/GAC及GAC在固定床实验装置中通入自来水进行TOC去除实验的差异。实验表明，负载TiO_2的活性炭提高了电催化再生吸附能力，负载量越高多次再生能力越强，从而降低经处理自来水中TOC的效果也越明显。
采用浸渍法在不同活性炭纤维材料(AFC)及泡沫镍上负载TiO_2，并以正交实验采用TiO_2在不同负载材料、层数、煅烧温度、硫酸、Fe~(3+)的加入量下制备吸附型光催化剂，用动态测试法研究各因数对苯的光催化降解率的影响。结果表明，TiO_2催化剂负载在ACF上，在一定质量浓度的TiO_2前驱溶胶中浸涂两层，250℃下煅烧一小时，加入适量的硫酸条件下对苯具有良好的降解性能；本研究中，最佳的掺杂铁离子量是0.10％。所制备样品的光催化降解苯的速率也符合Langmurir-Hinshelwoood的假一级动力学方程，吸附为控制步骤。
In the current work, the influence on preparing condition using the different large surface area material as supports, such as granular actived carbons and actived carbon fibers to the photocatalytic degradation performance activity have been investigated. Some new progresses were expected in the practical applications of photocatalytic technology.
Fe~(3+) doped nanometer TiO_2 photocatalysts was prepared with different content ferric citrate and different opposite anions of Fe using the Ti(SO_4)_2 precipitation method. the precursor of TiO_2 was dried over steam bath at 80℃with ultrasonic wave, then was calcined to form the high photocatalytic activities of nanometer Fe~(3+) doped TiO_2. The photocatalyst acitivity results indicated that the optimum doping amount of iron ion when doping ferric citrate was 0.05 mole% under UV and solar light and the photocatlytic activity even higher than that of Degussa P25 TiO_2,Over 1% Fe content doped TiO_2 powders showed a strong absorption in whole range 350-500 nm and a red shift in the band gap but showed the weaker photocatalytic activity. SO_4~(2-) ion doping can improve the photocatalytic degradation of TiO_2 and have better activity than that of doped with other different kind inorganic anions of Fe~(3+) salt.
The photocatalyst acitivity of nanometer titanium dioxide/ carbon material (TiO_2/C) was prepared by dip-coating technique by means of orthogonal experimental method. The effects of the conditions of prepared TiO_2/C catalyst on the photoelectrocatalysis degradation of methyl orange solution was investigated. The result was obtained that the specific surface areas of supporter play a decisive role in the degradation efficiency of methyl orange. The nano-sized TiO_2 was supported on active carbon (AC) were prepared by means of orthogonal experimental method too. The result showed that main influencing factor of photocatalysis activity was the doping amount of B~(3+) and H_2SO_4, and the effect of Fe~(3+) was much less. The kinetics of this degradation reaction conform to the Langmiur-Hinshelwood pseudo-first order kinetics model very well, and the absorption of OM on the prepared catalyst surface was the controlling step in the whole degradation process.
The adsorption and regeneration characteristics of TiO_2 supported on granular activated carbon were studied by using the electrical catalytic degradation, using methylene blue as a model organic pollutant. At the room temperature and electric voltage of 80V, the relation between removal efficiency and the loaded mass of TiO_2 was measured. The TOC removal in tap water was also used to test the efficiency packed both TiO_2/GAC and GAC into a packed-bed reactor as an adsorbent and catalyst in the electrochemical reaction. The experimental results show that loaded TiO_2 on GAC enhanced the electrical catalytic adsorption and regeneration capacity. That is, the more mass was loaded, the better regenerating performance was got, and the best TOC removal was obtained when ratio of TiO_2 to GAC was 0.8:1.
The TiO_2 photocatalyst were prepared by using dip-coating technique adhered precursor of TiO_2 to active carbon fiber and porous nickel mesh. The effects of different prepared factors, such as different supported materials, the times of coating, the calcining temperature and the added amount of H_2SO_4 were studied in photocatalytic oxidation of Benzene. The result showed that the ACF loaded with precursor of TiO_2 should be coated two times, calcined for 1 hours at 250℃and added proper amount of H2SO4. In this study, the optimum Fe~(3+) doping amount was ontained at 0.10%. And the kinetics of this degradation reaction of Benzene also corform to the Langmiur-Hinshelwood pseudo-first order kinetics model very well.
引文
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