二氧化钛/分子筛复合催化剂的合成及其光催化臭氧耦合降解乙醛性能的研究
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摘要
随着生活水平的提高,人们对室内空气的质量要求也越来越高,空气净化的研究也逐渐成为人们所关注的热点。空气净化的方式有许多种,各有优缺点,例如:利用光催化降解有害气体,其优点是能耗低、操作简单、无二次污染;缺点是效率低、反应速度慢,且光催化剂易失活;臭氧氧化技术虽然氧化能力强,但臭氧本身也是污染物,会带来二次污染,且臭氧的氧化没有选择性,无法针对目标污染物进行选择性氧化,另外现有的臭氧氧化工艺比较复杂,初期投资及运行费用很高,操作工艺比较复杂。
近期利用光催化臭氧协同作用降解有机污染物也取得了一定进展,但主要是局限在反应物浓度、臭氧浓度、空气温湿度及紫外灯强度对降解的影响,而对于催化剂的负载量、晶型、载体材料类型、载体的孔结构及孔径分布以及载体的过渡金属离子改性对光催化臭氧降解的影响以及机理研究甚少,而这些研究对于提高光催化臭氧耦合降解污染物的效率是非常具有实验指导意义。空气中污染物浓度低,流速快,污染物不易在催化剂表面被氧化。因此,提高催化剂对空气中有机污染物的吸附和富集可以促进反应快速进行。分子筛是良好的吸附材料,尤其适合对有机小分子污染物的吸附。因此本文主要研究二氧化钛负载量、晶型、分子筛材料类型、孔径分布、孔径尺寸以及利用过渡金属对分子筛改性后对光催化臭氧降解污染物的影响及机理。其结论分述如下:
1.对负载二氧化钛的煤制活性炭与竹制活性炭的性能研究中发现,载体导电性会影响催化剂光催化性能,导电性能好的载体负载二氧化钛后的活性反而较差;另外载体的规整有序孔结构和孔径分布直接影响到臭氧氧化乙醛的效率;在光催化臭氧耦合体系中,臭氧在降解乙醛所起的作用较光催化更为明显,竹制活性炭为载体的催化剂对臭氧的利用率高,因此其光催化臭氧耦合对乙醛的降解效率更高。
2.在TiO2/MCM-41复合催化剂中,负载的二氧化钛晶体颗粒的分布量和形态直接影响到催化剂的活性,在保证载体有较高比表面积的前提下,具有适量、分布均匀且晶相合适的二氧化钛晶体颗粒是提高光催化活性的关键;在MCM-41上负载的TiO2可以改善其表面憎水性,增强对乙醛分子的吸附性能,增大了臭氧与乙醛分子的接触时间和机率,提高了臭氧的利用率。
3.臭氧浓度以及反应物与催化剂的接触时间将影响降解效率,臭氧浓度有利于降解效率的提高,气固两相的接触时间也会影响单位时间的降解量,如何在传质速率和表面反应速率之间找到平衡点,是提高单位时间降解量的关键。
4.通过对三种不同载体对比发现,择形吸附与催化剂载体的孔径尺寸、反应物分子半径及形状有关;择形吸附能大大提高载体对目标反应物的选择性吸附量,从而提高反应物在催化剂上的浓度,使得催化(光催化、臭氧氧化,或者两者的耦合催化)反应速率大大提高。通过对载体的紫外线的吸收性能与催化剂活性关系的研究结果表明,竹制活性炭对紫外线强烈吸收使得TiO2/BC在光催化以及光催化臭氧耦合下活性均不高,MCM-41和H-ZSM-5对紫外线的不吸收使得TiO2/MCM-41和TiO2/H-ZSM-5在光催化以及光催化臭氧耦合下的活性较高。
5.通过离子交换法得到了M-ZSM-5(M=Zn、Cu、Mn),并以此为载体合成了TiO2/M-ZSM-5系列催化剂。降解乙醛实验结果标明:在单一紫外灯照射下,M-ZSM-5均表现出一定的光催化活性,其活性顺序为: Cu-ZSM-5 >Zn-ZSM-5>Mn-ZSM-5。但在负载二氧化钛后,其光催化活性没有明显提高,TiO2/Zn-ZSM-5和TiO2/Cu-ZSM-5还出现下降。在单一臭氧条件下,M-ZSM-5和TiO2/M-ZSM-5均对乙醛有一定降解率,尤其以Mn-ZSM-5的活性最高,负载二氧化钛的M-ZSM-5的活性均比相应的M-ZSM-5低。在光催化臭氧耦合降解乙醛过程中,M-ZSM-5和TiO2/M-ZSM-5对乙醛的降解效率均比单一光催化或单一臭氧下高,其光催化臭氧耦合下的活性顺序为:TiO2/Mn-ZSM-5 >Mn-ZSM-5 >Cu-ZSM-5>TiO2/Cu-ZSM-5>Zn-ZSM-5>TiO2/Zn-ZSM-5。
6.在M-ZSM-5中(M=Zn、Cu、Mn),乙醛分子易于Zn、Cu、Mn离子结合形成了相对的稳定态,难以迁移到二氧化钛表面发生光催化降解,因此M-ZSM-5在负载二氧化钛后的光催化活性没有得到明显改善,甚至还有降低。Mn-ZSM-5在臭氧存在下对乙醛的降解率相比Zn-ZSM-5和Cu-ZSM-5要高,这是由于Mn离子易促使臭氧分解产生活性氧原子,因此对臭氧的利用率最高,但M-ZSM-5在负载二氧化钛后,降解率均略有下降,这可能是如下两个原因:一是比表面积下降,二是负载的二氧化钛覆盖部分过渡金属离子,使反应活性位减少。在光催化臭氧耦合条件下,乙醛降解率提高的原因一方面是由于紫外灯和臭氧在催化剂上直接氧化乙醛,另一方面产生的光生电子通过与臭氧分子反应产生大量的活性氧原子增强了对乙醛的降解作用。
Nowadays, indoor air quality is paid more and more attention with improvement of our living standard. Indoor air purification also gradually becomes hot issue. However, there are so many kinds of air purification methods, which have advantages and disadvantages. Photocatalytic is a new technology for degradation of pollution gas. Its advantages are low energy consumption, simple operation, no secondary pollution; disadvantages are low efficiency, low reaction rate, easily lost activity of catalyst. Ozone oxidation is another technology for removal of air pollution. However, ozone can bring about secondary pollution though it has strong oxidation ability, and ozonation is not selective, can not target selective oxidation of pollutants. At the same time, the operational processes of ozone oxidation for removal of pollution are complicated, and need high initial investment and operating costs. Recently the photo-degradation of organic pollutants with the assist of ozone has also made some progress, but mostly confined to the effect of the reactant concentration, ozone concentration, air temperature and humidity and UV light intensity on the degradation. Howvever, the researchs about the effect of the catalyst loading, catalyst crystal, support material, pore structure, pore size distribution of support and the support modified by transition metal ions on the degradation were few, as well as the mechanism of degradation. But these researchs were very important for improving the degradation efficiency. Low concentration of pollutants in the air flow rate quickly, and pollutants are not easily oxidized on the catalyst surface. Therefore, the increasing of adsorption and condensation of pollutants on catalysts could promote the degradation rate. Molecular sieves were good adsorption materials, especially suitable for the adsorption of small organic molecules. Therefore, this dissertation mainly focus on the effect of titanium dioxide load, titanium dioxide crystal, molecular sieve material type, pore size distribution, pore size and molecular sieve modified by transition metal ions on photocatalytic degradation of pollutants with the assist of ozone, as well as the degradation mechanism. The contents and conclusions are as follows: In comparison with the performance of activated carbon activated bamboo carbon with titianium dioxide loading, the following facts were found. First, the conductive property of support had effect on the photocatalysis of it. The better electrical conductivity of support is, the worse the photocatalytic activity of catalyst is. Second, the orderly pore structure and narrow distribution of pore was favorable to the increasing of ozone usage. Last, Ozone plays a more important role than photocatalysis under the condition of Uv-ozone. As to activated carbon and activated bamboo carbon, the acetaldehyde degradation on the latter is higher because of its ozone usage.
In the investigation of photo-degradation acetaldehyde on TiO2/MCM-41 composite catalysts assisted by ozone, it was found that distribution and crystal phase of TiO2 loading affected photocatalysis activity of catalysts. High photocatalysis activity of catalyst should be the result of high specific surface area, large amount of TiO2 loading and suitable phase of TiO2 loading. It also was found that TiO2 loading could enhance hydrophobic property of MCM-41, which was favorable to the adsorption of acetaldehyde on catalysts. The adsorption increment of acetaldehyde on catalyst could increase the contact time and probability between ozone with acetaldehyde molecular, which lead to the increasing of ozone usage.
The degradation efficiency of acetaldehyde was also influenced by the concentration of ozone and the contact time between reactants with catalysts. The gas-solid contact time also affected the rate of degradation capacity. Then, the key to increasing the rate of degradation capacity is how to find out balance between the rates of mass transfer with the rate of surface reaction. Selective adsorption was relative to pore size of molecular sieve and the radius and shape of reactant molecular through the comparison of three molecular sieves. The selective adsorption can enhance remarkably adsorption amount of target reactant on support, leading to the increasing of reactant concentration on catalyst, which can increase the degradation rate of acetaldehyde under UV lamp, ozone or UV-ozone. The absorbance of support to ultra-violet can also affect the photocatalytic activity of catalysts. The activity of TiO2/BC was low under the condition of UV lamp or UV-ozone because of the strong adsorption of activated bamboo carbon to ultra-violet, on the contrary, the activity of TiO2/MCM-41 and TiO2/H-ZSM-5 was higher because of the weak adsorption of MCM-41 or H-ZSM-5 to ultra-violet M-ZSM-5 (M=Zn、Cu、Mn)were prepared by ion-exchange method. TiO2/M-ZSM-5 serials of catalysts were synthesized by impregnation method. The conclusions could be drawn in the investigation of the degradation of acetaldehyde on M-ZSM-5 or TiO2/M-ZSM-5 as follows: M-ZSM-5 have shown a certain degree of photocatalytic activity under the condition of UV lamp. The activity of the order: Cu-ZSM-5>Zn-ZSM-5>Mn-ZSM-5. But the photocatalytic activity of TiO2/M-ZSM-5 has not greatly improved, and some actually declined. All M-ZSM-5 and TiO2/M-ZSM-5 catalysts have activity to degrade a certain amount of acetaldehyde under the condition of ozone, especially Mn-ZSM-5 own the highest activity. But the degradation efficiency decreased slightly on TiO2/M-ZSM-5 catalysts. All the sample of acetaldehyde degradation efficiency was higher under the condition UV-ozone than those under UV or ozone. The activity of the order under the condition of Uv-ozone: TiO2/Mn-ZSM-5>Mn-ZSM-5>Cu-ZSM-5 >TiO2/Cu-ZSM-5>Zn-ZSM-5>TiO2/Zn-ZSM-5. Acetaldehyde molecules interact easily with Zn, Cu, Mn ion to form a stable state in M-ZSM-5 (M= Zn, Cu, Mn), making it difficult to transfer to the surface of titanium dioxide to be photodegraded. Therefore the photocatalytic activities of M-ZSM-5 with titianium dioxide loading are not improved compare to M-ZSM-5, TiO2/Zn-ZSM-5 and TiO2/Cu-ZSM-5 also declined. Mn-ZSM-5 own the highest activity than the other catalysts under the condition of ozone because Mn ions can catalyze ozone to produce maximum amount of reactive oxygen atoms among the three transition metal ion, which make it has the maximum utilization of ozone. However, the acetaldehyde degradation declined after loading titianium dioxide due to the decreasing of specific surface area, and then also may be due to titanium dioxide loading, which would cover the part of the transition metal ions leading to the decline of reaction active sites. The increasing of acetaldehyde conversion under the condition Uv-ozone may be contributed by following factors. First, The UV light or ozone can degrade the acetaldehyde on catalysts directly. Second, the reaction between photo-generated electron and ozone can produce large amount reactive oxygen atoms to decompose acetaldehyde. Therefore, the photodegradation efficiency of acetaldehyde increased greatly with the assistance of ozone, although the photocatalytic activity of M-ZSM-5 or TiO2/M-ZSM-5 is low.
近期利用光催化臭氧协同作用降解有机污染物也取得了一定进展,但主要是局限在反应物浓度、臭氧浓度、空气温湿度及紫外灯强度对降解的影响,而对于催化剂的负载量、晶型、载体材料类型、载体的孔结构及孔径分布以及载体的过渡金属离子改性对光催化臭氧降解的影响以及机理研究甚少,而这些研究对于提高光催化臭氧耦合降解污染物的效率是非常具有实验指导意义。空气中污染物浓度低,流速快,污染物不易在催化剂表面被氧化。因此,提高催化剂对空气中有机污染物的吸附和富集可以促进反应快速进行。分子筛是良好的吸附材料,尤其适合对有机小分子污染物的吸附。因此本文主要研究二氧化钛负载量、晶型、分子筛材料类型、孔径分布、孔径尺寸以及利用过渡金属对分子筛改性后对光催化臭氧降解污染物的影响及机理。其结论分述如下:
1.对负载二氧化钛的煤制活性炭与竹制活性炭的性能研究中发现,载体导电性会影响催化剂光催化性能,导电性能好的载体负载二氧化钛后的活性反而较差;另外载体的规整有序孔结构和孔径分布直接影响到臭氧氧化乙醛的效率;在光催化臭氧耦合体系中,臭氧在降解乙醛所起的作用较光催化更为明显,竹制活性炭为载体的催化剂对臭氧的利用率高,因此其光催化臭氧耦合对乙醛的降解效率更高。
2.在TiO2/MCM-41复合催化剂中,负载的二氧化钛晶体颗粒的分布量和形态直接影响到催化剂的活性,在保证载体有较高比表面积的前提下,具有适量、分布均匀且晶相合适的二氧化钛晶体颗粒是提高光催化活性的关键;在MCM-41上负载的TiO2可以改善其表面憎水性,增强对乙醛分子的吸附性能,增大了臭氧与乙醛分子的接触时间和机率,提高了臭氧的利用率。
3.臭氧浓度以及反应物与催化剂的接触时间将影响降解效率,臭氧浓度有利于降解效率的提高,气固两相的接触时间也会影响单位时间的降解量,如何在传质速率和表面反应速率之间找到平衡点,是提高单位时间降解量的关键。
4.通过对三种不同载体对比发现,择形吸附与催化剂载体的孔径尺寸、反应物分子半径及形状有关;择形吸附能大大提高载体对目标反应物的选择性吸附量,从而提高反应物在催化剂上的浓度,使得催化(光催化、臭氧氧化,或者两者的耦合催化)反应速率大大提高。通过对载体的紫外线的吸收性能与催化剂活性关系的研究结果表明,竹制活性炭对紫外线强烈吸收使得TiO2/BC在光催化以及光催化臭氧耦合下活性均不高,MCM-41和H-ZSM-5对紫外线的不吸收使得TiO2/MCM-41和TiO2/H-ZSM-5在光催化以及光催化臭氧耦合下的活性较高。
5.通过离子交换法得到了M-ZSM-5(M=Zn、Cu、Mn),并以此为载体合成了TiO2/M-ZSM-5系列催化剂。降解乙醛实验结果标明:在单一紫外灯照射下,M-ZSM-5均表现出一定的光催化活性,其活性顺序为: Cu-ZSM-5 >Zn-ZSM-5>Mn-ZSM-5。但在负载二氧化钛后,其光催化活性没有明显提高,TiO2/Zn-ZSM-5和TiO2/Cu-ZSM-5还出现下降。在单一臭氧条件下,M-ZSM-5和TiO2/M-ZSM-5均对乙醛有一定降解率,尤其以Mn-ZSM-5的活性最高,负载二氧化钛的M-ZSM-5的活性均比相应的M-ZSM-5低。在光催化臭氧耦合降解乙醛过程中,M-ZSM-5和TiO2/M-ZSM-5对乙醛的降解效率均比单一光催化或单一臭氧下高,其光催化臭氧耦合下的活性顺序为:TiO2/Mn-ZSM-5 >Mn-ZSM-5 >Cu-ZSM-5>TiO2/Cu-ZSM-5>Zn-ZSM-5>TiO2/Zn-ZSM-5。
6.在M-ZSM-5中(M=Zn、Cu、Mn),乙醛分子易于Zn、Cu、Mn离子结合形成了相对的稳定态,难以迁移到二氧化钛表面发生光催化降解,因此M-ZSM-5在负载二氧化钛后的光催化活性没有得到明显改善,甚至还有降低。Mn-ZSM-5在臭氧存在下对乙醛的降解率相比Zn-ZSM-5和Cu-ZSM-5要高,这是由于Mn离子易促使臭氧分解产生活性氧原子,因此对臭氧的利用率最高,但M-ZSM-5在负载二氧化钛后,降解率均略有下降,这可能是如下两个原因:一是比表面积下降,二是负载的二氧化钛覆盖部分过渡金属离子,使反应活性位减少。在光催化臭氧耦合条件下,乙醛降解率提高的原因一方面是由于紫外灯和臭氧在催化剂上直接氧化乙醛,另一方面产生的光生电子通过与臭氧分子反应产生大量的活性氧原子增强了对乙醛的降解作用。
Nowadays, indoor air quality is paid more and more attention with improvement of our living standard. Indoor air purification also gradually becomes hot issue. However, there are so many kinds of air purification methods, which have advantages and disadvantages. Photocatalytic is a new technology for degradation of pollution gas. Its advantages are low energy consumption, simple operation, no secondary pollution; disadvantages are low efficiency, low reaction rate, easily lost activity of catalyst. Ozone oxidation is another technology for removal of air pollution. However, ozone can bring about secondary pollution though it has strong oxidation ability, and ozonation is not selective, can not target selective oxidation of pollutants. At the same time, the operational processes of ozone oxidation for removal of pollution are complicated, and need high initial investment and operating costs. Recently the photo-degradation of organic pollutants with the assist of ozone has also made some progress, but mostly confined to the effect of the reactant concentration, ozone concentration, air temperature and humidity and UV light intensity on the degradation. Howvever, the researchs about the effect of the catalyst loading, catalyst crystal, support material, pore structure, pore size distribution of support and the support modified by transition metal ions on the degradation were few, as well as the mechanism of degradation. But these researchs were very important for improving the degradation efficiency. Low concentration of pollutants in the air flow rate quickly, and pollutants are not easily oxidized on the catalyst surface. Therefore, the increasing of adsorption and condensation of pollutants on catalysts could promote the degradation rate. Molecular sieves were good adsorption materials, especially suitable for the adsorption of small organic molecules. Therefore, this dissertation mainly focus on the effect of titanium dioxide load, titanium dioxide crystal, molecular sieve material type, pore size distribution, pore size and molecular sieve modified by transition metal ions on photocatalytic degradation of pollutants with the assist of ozone, as well as the degradation mechanism. The contents and conclusions are as follows: In comparison with the performance of activated carbon activated bamboo carbon with titianium dioxide loading, the following facts were found. First, the conductive property of support had effect on the photocatalysis of it. The better electrical conductivity of support is, the worse the photocatalytic activity of catalyst is. Second, the orderly pore structure and narrow distribution of pore was favorable to the increasing of ozone usage. Last, Ozone plays a more important role than photocatalysis under the condition of Uv-ozone. As to activated carbon and activated bamboo carbon, the acetaldehyde degradation on the latter is higher because of its ozone usage.
In the investigation of photo-degradation acetaldehyde on TiO2/MCM-41 composite catalysts assisted by ozone, it was found that distribution and crystal phase of TiO2 loading affected photocatalysis activity of catalysts. High photocatalysis activity of catalyst should be the result of high specific surface area, large amount of TiO2 loading and suitable phase of TiO2 loading. It also was found that TiO2 loading could enhance hydrophobic property of MCM-41, which was favorable to the adsorption of acetaldehyde on catalysts. The adsorption increment of acetaldehyde on catalyst could increase the contact time and probability between ozone with acetaldehyde molecular, which lead to the increasing of ozone usage.
The degradation efficiency of acetaldehyde was also influenced by the concentration of ozone and the contact time between reactants with catalysts. The gas-solid contact time also affected the rate of degradation capacity. Then, the key to increasing the rate of degradation capacity is how to find out balance between the rates of mass transfer with the rate of surface reaction. Selective adsorption was relative to pore size of molecular sieve and the radius and shape of reactant molecular through the comparison of three molecular sieves. The selective adsorption can enhance remarkably adsorption amount of target reactant on support, leading to the increasing of reactant concentration on catalyst, which can increase the degradation rate of acetaldehyde under UV lamp, ozone or UV-ozone. The absorbance of support to ultra-violet can also affect the photocatalytic activity of catalysts. The activity of TiO2/BC was low under the condition of UV lamp or UV-ozone because of the strong adsorption of activated bamboo carbon to ultra-violet, on the contrary, the activity of TiO2/MCM-41 and TiO2/H-ZSM-5 was higher because of the weak adsorption of MCM-41 or H-ZSM-5 to ultra-violet M-ZSM-5 (M=Zn、Cu、Mn)were prepared by ion-exchange method. TiO2/M-ZSM-5 serials of catalysts were synthesized by impregnation method. The conclusions could be drawn in the investigation of the degradation of acetaldehyde on M-ZSM-5 or TiO2/M-ZSM-5 as follows: M-ZSM-5 have shown a certain degree of photocatalytic activity under the condition of UV lamp. The activity of the order: Cu-ZSM-5>Zn-ZSM-5>Mn-ZSM-5. But the photocatalytic activity of TiO2/M-ZSM-5 has not greatly improved, and some actually declined. All M-ZSM-5 and TiO2/M-ZSM-5 catalysts have activity to degrade a certain amount of acetaldehyde under the condition of ozone, especially Mn-ZSM-5 own the highest activity. But the degradation efficiency decreased slightly on TiO2/M-ZSM-5 catalysts. All the sample of acetaldehyde degradation efficiency was higher under the condition UV-ozone than those under UV or ozone. The activity of the order under the condition of Uv-ozone: TiO2/Mn-ZSM-5>Mn-ZSM-5>Cu-ZSM-5 >TiO2/Cu-ZSM-5>Zn-ZSM-5>TiO2/Zn-ZSM-5. Acetaldehyde molecules interact easily with Zn, Cu, Mn ion to form a stable state in M-ZSM-5 (M= Zn, Cu, Mn), making it difficult to transfer to the surface of titanium dioxide to be photodegraded. Therefore the photocatalytic activities of M-ZSM-5 with titianium dioxide loading are not improved compare to M-ZSM-5, TiO2/Zn-ZSM-5 and TiO2/Cu-ZSM-5 also declined. Mn-ZSM-5 own the highest activity than the other catalysts under the condition of ozone because Mn ions can catalyze ozone to produce maximum amount of reactive oxygen atoms among the three transition metal ion, which make it has the maximum utilization of ozone. However, the acetaldehyde degradation declined after loading titianium dioxide due to the decreasing of specific surface area, and then also may be due to titanium dioxide loading, which would cover the part of the transition metal ions leading to the decline of reaction active sites. The increasing of acetaldehyde conversion under the condition Uv-ozone may be contributed by following factors. First, The UV light or ozone can degrade the acetaldehyde on catalysts directly. Second, the reaction between photo-generated electron and ozone can produce large amount reactive oxygen atoms to decompose acetaldehyde. Therefore, the photodegradation efficiency of acetaldehyde increased greatly with the assistance of ozone, although the photocatalytic activity of M-ZSM-5 or TiO2/M-ZSM-5 is low.
引文
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