多金属氧酸盐/TiO_2（WO_3）复合催化剂光解水催化性能研究
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摘要
设计和合成高效光催化剂是利用太阳能光催化分解水制氢的关键。本论文重点研究了二氧化钛和三氧化钨负载多金属氧酸盐(H_4SiW_(12)O_(40)和H_4PW_(12)O_(40))及负载对多金属氧酸盐光催化活性的影响:
采用溶胶-凝胶结合浸渍合成技术,制备了具有较高紫外光催化活性的负载型多金属氧酸盐纳米材料:H_4SiW_(12)O_(40)╱TiO_2、H_4PW_(12)O_(40)╱TiO_2,通过采用XRD、EDS、FT-IR、Raman、UV-DRS等手段对上述新材料进行了组成测定和结构表征,研究了在紫外光源照射下,POM/TiO_2复合催化材料光催化分解水的析氧率、反应机理。结果表明:母体POM基本骨架结构仍得以保留,POM/TiO_2在紫外范围内具有强烈的光吸收性能。当TiO_2为锐钛矿相、焙烧温度为250℃、焙烧时间为3h、质量比w(TiO_2):w(POM)为1:10的POM/TiO_2光催化剂活性最高,H_4SiW_(12)O_(40)/TiO_2的最佳析氧率为269.94μmol·l~(-1)·h~(-1),是H_4SiW_(12)O_(40)的1.4倍,TiO_2的4.5倍;H_4PW_(12)O_(40)╱TiO_2的最佳析氧率为199.95μmol·l~(-1)·h~(-1),是H_4PW_(12)O_(40)的1.9倍,约为TiO_2的3倍。POM和TiO_2之间存在良好的协同效应。
利用固相烧结和浸渍法相结合的技术合成了两种多金属氧酸盐/三氧化钨复合催化材料:H_4SiW_(12)O_(40)/WO_3和H_4PW_(12)O_(40)/WO_3,利用XRD、FT-IR、Raman、UV-DRS对制备所得产物进行了表征,并研究了该类新型复合催化剂在紫外光源照射下,光催化分解水析氧的催化性能。结果表明,在POM╱WO_3中,多金属氧酸盐的基本结构仍然完整,由于与载体WO_3之间存在着较强的吸附作用,致使POM/WO_3的谱线发生移动,峰强发生变化;焙烧时间、焙烧温度、质量比w(WO_3):w(POM)和电子受体Fe~(3+)的浓度等因素对POM/WO_3复合催化剂光催化分解水析氧的催化性能均有影响。电子受体Fe~(3+)的浓度为5g╱L,质量比w(WO_3):w(H_4SiW_(12)O_(40))为1:10的H_4SiW_(12)O_(40)╱WO_3复合催化剂在400℃下焙烧3h时光催化活性最佳,析氧率为143.13μmol·l~(-1)·h~(-1),但仍然没有H_4SiW_(12)O_(40)的析氧率高;电子受体Fe~(3+)的浓度为5g╱L,质量比w(WO_3)/w(H_4PW_(12)O_(40))为1:5的H_4PW_(12)O_(40)╱WO_3复合催化剂在400℃下焙烧3h时光催化活性最佳,析氧率为114.50μmol·l~(-1)·h~(-1),略高于H_4PW_(12)O_(40)的析氧率。
Design and synthesis of high efficient photocatalyst is significant for solar hydrogen.This research focuses on preparation and characterization of polyoxometallate supported TiO_2 or WO_3 photocatysts for water splitting.Some innovative results are as follows:
Polyoxometallate supported catalysts such as H_4SiW_(12)O_(40)/TiO_2、H_4PW_(12)O_(40)/TiO_2,with a high activity under ultraviolet radiation were prepared by sol-gel technology and impregnation methods.Samples were characterized by XRD,EDS,FT-IR,Raman and UV-DRS.Oxygen production rate and reaction mechanism of POM/TiO_2 composite catalysts were investigated.The results indicate that original structure of POM was retained and POM/TiO_2 showed a strong capacity in absorbing ultraviolet.Moreover,as titanium dioxide was in anatase phase,the calcination temperature and time was 250℃and 3h respectively,the mass ratio of TiO_2 to POM was 1:10,the photocatalytic activity reached the top, the fastest oxygen production rate of H_4SiW_(12)O_(40)/TiO_2 was 269.94μmol·l~(-1)·h~(-1),which was 1.4 times to that of H_4SiW_(12)O_(40),and 4.5 times TiO_2,which showed synergetic effect existed between POM and TiO_2.
Two kinds of POM/WO_3 composite catalysts,H_4SiW_(12)O_(40)/WO_3 and H_4PW_(12)O_(40)/WO_3 were prepared by solid-state sintering method and impregnation.XRD,FT-IR,Raman,UV-DRS were applied to characterize their structure and their photocatalytic performance in oxygen production for water splitting under ultraviolet.The result showed that catalysts were in nano size.For POM/WO_3,original structure of POM didn't change significantly.Because of the physical interaction between WO_3 and POM,IR spectra peak intensity of POM/WO_3 changed. Calcination time,temperature,mass ratio(w(WO_3):w(POM))and concentration of Fe~(3+)would affect performance of catalysts.As concentration of electron acceptors was 5g/L,and when the ratio(w (WO_3):w(H_4SiW_(12)O_(40)))was 1:10,calcination time and temperature was 3h and 400℃respectively,H_4SiW_(12)O_(40)/WO_3 composite catalyst exhibited the highest photocatalytic activity,and oxygen production rate was 143.13μmol·l~(-1)·h~(-1),however,this value was still lower than that of H_4SiW_(12)O_(40);when concentration of Fe~(3+)was 5g/L,mass ratio(w(WO_3) /w(H_4PW_(12)O_(40)))was 1:5,calcined for 3h under 400℃,the catalyst showed the best performance and oxygen production rate was 114.50μmol·l~(-1)·h~(-1),slightly higher than that of H_4PW_(12)O_(40).
采用溶胶-凝胶结合浸渍合成技术,制备了具有较高紫外光催化活性的负载型多金属氧酸盐纳米材料:H_4SiW_(12)O_(40)╱TiO_2、H_4PW_(12)O_(40)╱TiO_2,通过采用XRD、EDS、FT-IR、Raman、UV-DRS等手段对上述新材料进行了组成测定和结构表征,研究了在紫外光源照射下,POM/TiO_2复合催化材料光催化分解水的析氧率、反应机理。结果表明:母体POM基本骨架结构仍得以保留,POM/TiO_2在紫外范围内具有强烈的光吸收性能。当TiO_2为锐钛矿相、焙烧温度为250℃、焙烧时间为3h、质量比w(TiO_2):w(POM)为1:10的POM/TiO_2光催化剂活性最高,H_4SiW_(12)O_(40)/TiO_2的最佳析氧率为269.94μmol·l~(-1)·h~(-1),是H_4SiW_(12)O_(40)的1.4倍,TiO_2的4.5倍;H_4PW_(12)O_(40)╱TiO_2的最佳析氧率为199.95μmol·l~(-1)·h~(-1),是H_4PW_(12)O_(40)的1.9倍,约为TiO_2的3倍。POM和TiO_2之间存在良好的协同效应。
利用固相烧结和浸渍法相结合的技术合成了两种多金属氧酸盐/三氧化钨复合催化材料:H_4SiW_(12)O_(40)/WO_3和H_4PW_(12)O_(40)/WO_3,利用XRD、FT-IR、Raman、UV-DRS对制备所得产物进行了表征,并研究了该类新型复合催化剂在紫外光源照射下,光催化分解水析氧的催化性能。结果表明,在POM╱WO_3中,多金属氧酸盐的基本结构仍然完整,由于与载体WO_3之间存在着较强的吸附作用,致使POM/WO_3的谱线发生移动,峰强发生变化;焙烧时间、焙烧温度、质量比w(WO_3):w(POM)和电子受体Fe~(3+)的浓度等因素对POM/WO_3复合催化剂光催化分解水析氧的催化性能均有影响。电子受体Fe~(3+)的浓度为5g╱L,质量比w(WO_3):w(H_4SiW_(12)O_(40))为1:10的H_4SiW_(12)O_(40)╱WO_3复合催化剂在400℃下焙烧3h时光催化活性最佳,析氧率为143.13μmol·l~(-1)·h~(-1),但仍然没有H_4SiW_(12)O_(40)的析氧率高;电子受体Fe~(3+)的浓度为5g╱L,质量比w(WO_3)/w(H_4PW_(12)O_(40))为1:5的H_4PW_(12)O_(40)╱WO_3复合催化剂在400℃下焙烧3h时光催化活性最佳,析氧率为114.50μmol·l~(-1)·h~(-1),略高于H_4PW_(12)O_(40)的析氧率。
Design and synthesis of high efficient photocatalyst is significant for solar hydrogen.This research focuses on preparation and characterization of polyoxometallate supported TiO_2 or WO_3 photocatysts for water splitting.Some innovative results are as follows:
Polyoxometallate supported catalysts such as H_4SiW_(12)O_(40)/TiO_2、H_4PW_(12)O_(40)/TiO_2,with a high activity under ultraviolet radiation were prepared by sol-gel technology and impregnation methods.Samples were characterized by XRD,EDS,FT-IR,Raman and UV-DRS.Oxygen production rate and reaction mechanism of POM/TiO_2 composite catalysts were investigated.The results indicate that original structure of POM was retained and POM/TiO_2 showed a strong capacity in absorbing ultraviolet.Moreover,as titanium dioxide was in anatase phase,the calcination temperature and time was 250℃and 3h respectively,the mass ratio of TiO_2 to POM was 1:10,the photocatalytic activity reached the top, the fastest oxygen production rate of H_4SiW_(12)O_(40)/TiO_2 was 269.94μmol·l~(-1)·h~(-1),which was 1.4 times to that of H_4SiW_(12)O_(40),and 4.5 times TiO_2,which showed synergetic effect existed between POM and TiO_2.
Two kinds of POM/WO_3 composite catalysts,H_4SiW_(12)O_(40)/WO_3 and H_4PW_(12)O_(40)/WO_3 were prepared by solid-state sintering method and impregnation.XRD,FT-IR,Raman,UV-DRS were applied to characterize their structure and their photocatalytic performance in oxygen production for water splitting under ultraviolet.The result showed that catalysts were in nano size.For POM/WO_3,original structure of POM didn't change significantly.Because of the physical interaction between WO_3 and POM,IR spectra peak intensity of POM/WO_3 changed. Calcination time,temperature,mass ratio(w(WO_3):w(POM))and concentration of Fe~(3+)would affect performance of catalysts.As concentration of electron acceptors was 5g/L,and when the ratio(w (WO_3):w(H_4SiW_(12)O_(40)))was 1:10,calcination time and temperature was 3h and 400℃respectively,H_4SiW_(12)O_(40)/WO_3 composite catalyst exhibited the highest photocatalytic activity,and oxygen production rate was 143.13μmol·l~(-1)·h~(-1),however,this value was still lower than that of H_4SiW_(12)O_(40);when concentration of Fe~(3+)was 5g/L,mass ratio(w(WO_3) /w(H_4PW_(12)O_(40)))was 1:5,calcined for 3h under 400℃,the catalyst showed the best performance and oxygen production rate was 114.50μmol·l~(-1)·h~(-1),slightly higher than that of H_4PW_(12)O_(40).
引文
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