CN106799222B - 一种二氧化钛/铌酸锡复合纳米材料的制备方法 - Google Patents
一种二氧化钛/铌酸锡复合纳米材料的制备方法 Download PDFInfo
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- 239000002253 acid Substances 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 12
- 239000010955 niobium Substances 0.000 title claims abstract description 12
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- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 3
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明涉及一种二氧化钛/铌酸锡复合纳米材料的制备方法，属于材料制备和光催化的技术领域。称取SnNb2O6纳米片溶于无水乙醇中，超声分散，再加入钛酸四丁酯(TBT)、去离子水，磁力搅拌，将溶液转移至内衬为聚四氟乙烯的反应釜中，将反应釜放入烘箱中，水热反应，待自然冷却至室温后，离心出浅黄色颗粒，水洗和醇洗后离心，烘干得到所述TiO2/SnNb2O6复合材料。本发明制备TiO2/SNO复合材料的反应工艺简单，所得产品光催化活性好，稳定性高，生产过程绿色环保。
Description
技术领域
本发明涉及一种二氧化钛/铌酸锡复合纳米材料的制备方法，属于材料制备和光催化的技术领域。
技术背景
近年来，由于光驱动半导体光催化材料在有机污染物降解、光解水、太阳能转化和环境进化等普遍应用，寻找和优化高效光催化剂已经引起人们极大的兴趣。到目前为止，大量半导体光催化材料如二氧化钛(TiO2)、硫化铬(CdS)、氧化锌(ZnO)、氧化钨(WO3)已经成功制备，并且被验证具有光催化活性。在众多半导体中，TiO2无毒、廉价、结构稳定，具有优良的光催化性能，是近年研究较多的半导体光催化剂之一。但是由于其禁带较宽(3.2eV)，仅能在紫外光区响应，而波长小于380nm的紫外光对应的能量仅占整个太阳能光谱波长范围总能量的3.39％，因此，TiO2能量利用率低；另外，TiO2光生电子-空穴容易复合，光催化效率有待提高。由此许多修饰TiO2半导体催化剂的方法相继产生，改性研究主要有金属/非金属元素掺杂、贵金属沉积、光敏化、结构调控及与其他半导体复合等，其中与其他半导体光催化材料复合构建异质结是最简单高效的方法，能有效的促进光生电子和空穴的分离，抑制光生电子与空穴的复合，提高光电转化的效率，扩展TiO2的吸收范围，从而提高光催化效率。
铌酸锡(SnNb2O6)作为典型的层状铌酸盐半导体材料，由于其独特的晶体结构和合适的能带结构在光催化分解水制氢和光降解有机污染物领域受到广泛关注。Wu以Nb2O5·nH2O为前驱体，通过微波辅助水热法制得SnNb2O6纳米片，有效的提高在可见光下降解RhB的效率。Chao Zhou等通过更为简便的水热法制备出厚度为3nm的超薄纳米片，与传统固相反应所制备的SnNb2O6颗粒相比，这种超薄纳米片具有极佳的降解和制氢效率。Lan Yuan等通过一个简单的表面电荷修饰的自组装方法合成二维SnNb2O6/石墨烯(GR)纳米复合材料，提高光生载流子有效的分离和转移，与单纯的SnNb2O6、GR相比，光催化活性大大提升。实验证明由于SnNb2O6具有优异的光催化性能,是光催化研究领域值得深入探索和研究的方向之一。
迄今为止，尚未发现有人采用水热法制备TiO2/SnNb2O6复合材料，所用的SNO化学和物理性质稳定，原材料廉价易得，无毒，且以其为载体制备TiO2/SNO复合材料的反应工艺简单，所得产品光催化活性好，稳定性高，生产过程绿色环保。
发明内容
本发明目的是提供一种新的在室温条件下，以简单易行的水热沉淀法合成TiO2/SnNb2O6复合材料的方法。
本发明通过以下步骤实现：
(1)制备铌酸锡(SnNb2O6)纳米片：称取五氧化二铌，氢氧化钾于内衬为聚四氟乙烯的反应釜中，向其中加入去离子水，然后将反应釜放入烘箱中，第一次水热反应；待自然冷却至室温后，得到澄清前驱体溶液，用稀盐酸调节溶液pH值，再加入二水合氯化亚锡，再次用稀盐酸调节pH值，将溶液转移至内衬为聚四氟乙烯的反应釜中，将反应釜放入烘箱中，第二次水热反应，待自然冷却至室温后，离心出黄色颗粒，水洗和醇洗数次，离心，烘干；具体可参考Z.Y.Zhang,D.L.Jiang,D.Li,M.He,M.Chen,Appl.Catal.B:Environ.183(2016)113-123。
所述第一次水热反应的温度为180℃，反应时间为48h。
所述稀盐酸溶液的浓度为2mol·L-1。
所述第二次水热反应的温度为200℃，反应时间为48h。
(2)称取SnNb2O6纳米片溶于无水乙醇中，超声分散，再加入钛酸四丁酯(TBT)、去离子水，磁力搅拌，将溶液转移至内衬为聚四氟乙烯的反应釜中，将反应釜放入烘箱中，水热反应，待自然冷却至室温后，离心出浅黄色颗粒，水洗和醇洗后离心，烘干得到所述TiO2/SnNb2O6复合材料；颗粒状的TiO2分散在SNO纳米片上。
所述超声分散指采用功率为250W的超声机超声30-60min。
所述磁力搅拌的时间为20min。
所述水热反应的温度为180℃，反应时间为12h。
所述烘干指于真空烘箱中60℃真空干燥12h。
所述无水乙醇、钛酸四丁酯和去离子水的体积比为：400：2：1。
所述TiO2/SnNb2O6复合材料中TiO2与SnNb2O6的质量比为0.1-0.5:1；优选0.2:1。
利用X射线衍射仪(XRD)、透射电子显微镜(TEM)、对产物进行形貌结构分析，以罗丹明B(RhB)溶液为目标染料进行光催化降解实验，通过紫外-可见分光光度计测量吸光度，以评估其光催化活性。
附图说明
图1为所制备单纯TiO2、SnNb2O6、TiO2/SnNb2O6复合材料的XRD衍射谱图；从图中可以看出不同质量比的TiO2/SnNb2O6的XRD图谱主要由TiO2和SnNb2O6的衍射峰构成，且随着TiO2质量分数的增加，TiO2的衍射峰越来越明显。
图2为所制备单纯TiO2、SnNb2O6、TiO2/SnNb2O6复合材料样品的透射电镜照片；图2a为单纯SnNb2O6透射电镜图；图2b为单纯TiO2透射电镜图；图2c-2g分别为10％-50％TiO2/SnNb2O6透射电镜图；图2h为20％TiO2/SnNb2O6高分辨透射电镜图；从图中可以看出超细TiO2颗粒(平均粒径为9.25nm)相对均匀的分散在SnNb2O6薄片表面。
图3为不同质量比的TiO2/SnNb2O6复合材料光催化降解RhB溶液的的时间-降解率关系图，从图中可以看出20％TiO2/SnNb2O6复合材料具有最高的光催化活性。
具体实施方式
实施例1 SnNb2O6纳米片的制备
SnNb2O6的制备采用的是水热反应的方法：称取0.5g五氧化二铌、2.2443g氢氧化钾于50mL内衬为聚四氟乙烯的反应釜中，向其中加入35mL去离子水，将反应釜放入烘箱，180℃水热反应48h，待自然冷却至室温后，得到澄清前驱体溶液，将溶液转移至50mL烧杯中，用浓度为2mol/L稀盐酸调节溶液pH至8，再加入0.4245g二水合氯化亚锡，磁力搅拌10min，再次用浓度为2mol/L稀盐酸调节溶液pH至2，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，200℃水热反应48h，冷却至室温，离心得到黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h。
实施例2 10％TiO2/SnNb2O6复合材料的制备
TiO2/SnNb2O6复合材料的制备采用的是水热沉淀法：称取0.423g SnNb2O6粉末溶于40mL无水乙醇中，然后在功率为250W的超声机中超声60min，再加入0.2mL TBT、0.1mL去离子水，磁力搅拌20min，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，180℃水热反应12h，冷却至室温，离心得到浅黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h，得到10％TiO2/SnNb2O6复合材料。
实施例3 20％TiO2/SnNb2O6复合材料的制备
TiO2/SnNb2O6复合材料的制备采用的是水热沉淀法：称取0.188g SnNb2O6粉末溶于40mL无水乙醇中，然后在功率为250W的超声机中超声60min，再加入0.2mL TBT、0.1mL去离子水，磁力搅拌20min，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，180℃水热反应12h，冷却至室温，离心得到浅黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h，得到20％TiO2/SnNb2O6复合材料。
实施例4 30％TiO2/SnNb2O6复合材料的制备
TiO2/SnNb2O6复合材料的制备采用的是水热沉淀法：称取0.1095g SnNb2O6粉末溶于40mL无水乙醇中，然后在功率为250W的超声机中超声50min，再加入0.2mL TBT、0.1mL去离子水，磁力搅拌20min，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，180℃水热反应12h，冷却至室温，离心得到浅黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h，得到30％TiO2/SnNb2O6复合材料。
实施例5 40％TiO2/SnNb2O6复合材料的制备
TiO2/SnNb2O6复合材料的制备采用的是水热沉淀法：称取0.0705g SnNb2O6粉末溶于40mL无水乙醇中，然后在功率为250W的超声机中超声40min，再加入0.2mL TBT、0.1mL去离子水，磁力搅拌20min，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，180℃水热反应12h，冷却至室温，离心得到浅黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h，得到40％TiO2/SnNb2O6复合材料。
实施例6 50％TiO2/SnNb2O6复合材料的制备
TiO2/SnNb2O6复合材料的制备采用的是水热沉淀法：称取0.047g SnNb2O6粉末溶于40mL无水乙醇中，然后在功率为250W的超声机中超声30min，再加入0.2mL TBT、0.1mL去离子水，磁力搅拌20min，将溶液转移至100mL内衬为聚四氟乙烯的反应釜中，放入烘箱，180℃水热反应12h，冷却至室温，离心得到浅黄色颗粒，水洗和醇洗各三次，离心，于真空烘箱中60℃真空干燥12h，得到50％TiO2/SnNb2O6复合材料。
实施例7不同比例TiO2/SnNb2O6复合光催化剂的光催化活性实验
(1)配制浓度为10mg/L的RhB溶液，将配好的溶液置于暗处。
(2)称取不同质量比的TiO2/SnNb2O6复合材料0.05g，分别置于光催化反应器中，加入50mL步骤(1)所配好的目标降解液，磁力搅拌30min待TiO2/SnNb2O6复合材料分散均匀后，打开水源，光源，进行光催化降解实验。
(3)每30min吸取反应器中的光催化降解液，离心后用于紫外-可见吸光度的测量。
(4)由图3可见所制备的20％TiO2/SnNb2O6复合材料具有优异的光催化活性，尤其是20％TiO2/SnNb2O6的样品在催化反应90min后RhB溶液降解率达到100％。
Claims (8)
1.一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：称取SnNb2O6纳米片溶于无水乙醇中，超声分散，再加入钛酸四丁酯、去离子水，磁力搅拌，将溶液转移至内衬为聚四氟乙烯的反应釜中，将反应釜放入烘箱中，水热反应，待自然冷却至室温后，离心出浅黄色颗粒，水洗和醇洗后离心，烘干得到所述TiO2/SnNb2O6复合材料；所述水热反应的温度为180℃，反应时间为12h。
2.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述TiO2/SnNb2O6复合材料，颗粒状的TiO2分散在SNO纳米片上。
3.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述超声分散指采用功率为250 W的超声机超声30-60min。
4.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述磁力搅拌的时间为20min。
5.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述烘干指于真空烘箱中60℃真空干燥12h。
6.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述无水乙醇、钛酸四丁酯和去离子水的体积比为：400：2：1。
7.如权利要求1所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述TiO2/SnNb2O6复合材料中，TiO2与SnNb2O6的质量比为0.1-0.5:1。
8.如权利要求7所述的一种二氧化钛/铌酸锡复合纳米材料的制备方法，其特征在于：所述TiO2/SnNb2O6复合材料中，TiO2与SnNb2O6的质量比为0.2:1。
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