CN106238049B - 一种Ag掺杂3DOM CeO2-ZrO2材料的制备 - Google Patents
一种Ag掺杂3DOM CeO2-ZrO2材料的制备 Download PDFInfo
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Abstract
本发明公开了一种通过减压填充合成方法制备Ag掺杂3DOM CeO2‑ZrO2复合光催化剂，属于化工行业技术领域。以聚苯乙烯(PS)胶球为大孔模板剂，并且以EO20PO70O20(P123)为介孔模板剂，采用Zr(OC4H9)4、Ce(NO3)3·6H2O、AgNO3为原料，通过减压填充后，经过干燥和煅烧得到3DOM Ag/CeO2‑ZrO2复合光催化剂。对其表面形貌、微观结构、光催化活性进行了测定，产品性能在降解刚果红和光解水制氢的光催化方面有很大提高。
Description
技术领域
本发明涉及一种减压填充方法制备的Ag掺杂3DOM CeO2-ZrO2复合光催化剂，属于化工行业技术领域。
背景技术
随着能源的消耗，利用太阳能分解水制氢的技术已经引起人们的广泛关注，而环境问题也成为经济发展的因素之一。新型光催化技术由于其对环境友好等特点引起了各国科学家的广泛关注。光催化技术大都以半导体材料为光催化剂，在光的激发下能够降解污染物。然而，一般光催化剂存在对太阳光的利用率较低等缺点，所以制备高效光催化材料在光解水制氢及降解污染物方面显得非常有意义。
发明内容
为了解决上述问题，本发明的目的在于提供一种减压填充法合成Ag掺杂3DOMCeO2-ZrO2复合光催化剂，一是由于CeO2和ZrO2都具有合适的带隙位置，能够利用光分解水产生氢气。二，通过制备三维有序大孔复合材料(3DOM)能够扩大材料的比表面积，增加反应的活性位点，同时，3DOM通透开放的大孔结构能够降低物质的传质阻力，有利于反应物分子的扩散。三，通过Ag的掺杂能够使催化的光响应范围拓宽至可见光区，提高光催化剂对太阳光的利用率，并且Ag的掺杂增加了复合材料光生电子的迁移途径，这种光生电子的多途径迁移从本质上降低了光生电子-空穴对的复合率，提高了复合材料的光催化反应效率。以聚苯乙烯(PS)胶球为大孔模板剂，并且以EO20PO70O20(P123)为介孔模板剂，采用Zr(OC4H9)4、Ce(NO3)3·6H2O、AgNO3为原料，通过减压填充后，经过干燥和煅烧得到3DOM Ag/CeO2-ZrO2复合光催化剂。
本发明解决其技术问题所采用的技术方案是：减压填充法合成Ag掺杂3DOM CeO2-ZrO2复合光催化剂，称取P123，质量为0.050±0.005 g，异丙醇(IPA)，体积为17 mL，PS，质量为0.500±0.010 g，Zr(OC4H9)4，体积为1.5 mL，Ce(NO3)3·6H2O，质量为0.167±0.002 g，AgNO3，质量为0.023±0.001 g。Ce(NO3)3·6H2O与AgNO3溶解于2 mL IPA中备用。将P123加入到IPA中并搅拌至完全溶解后滴加Zr(OC4H9)4，随后加入Ce(NO3)3与AgNO3溶液至形成Ag/CeO2-ZrO2溶胶，将PS模板置于Ag/CeO2-ZrO2溶胶中，搅拌一段时间后进行减压填充。将产物放入烘箱中至干燥，设定烘干温度60±2 ℃，干燥后所获产物在600 ℃下煅烧7 h，得到三维有序大孔复合材料Ag/CeO2-ZrO2 (标记为3DOM Ag/CeO2-ZrO2)。
本发明的有益效果是：采用减压填充法合成具有较高可见光响应的3DOM Ag/CeO2-ZrO2复合光催化剂。复合材料由立方相Ag、立方相CeO2和四方相ZrO2组成，且Ag的引入提高了光催化剂在可见光区的吸收。3DOM Ag/CeO2-ZrO2具有的三维有序大孔结构使材料具有较大的比表面积。与P25相比，复合光催化剂在模拟日光和可见光下对刚果红具有较好的光降解效果。另外，复合催化剂在Na2S-Na2SO3为牺牲剂的条件下具有较高的产氢效果，这是由于Ag的引入，扩大了复合材料可见光响应的范围，同时增加了光生电子的迁移途径，抑制了复合材料中光生电子-空穴对的复合，从而改善其光催化活性。
附图说明
下面结合附图和具体实施方式对本发明做进一步说明。
图1是PS胶晶模板表面形貌图。
图2是3DOM Ag/CeO2-ZrO2复合光催化剂表面形貌图。
图3是3DOM Ag/CeO2-ZrO2复合光催化剂的HR-TEM照片。
图4是3DOM Ag/CeO2-ZrO2复合光催化剂的XRD图。
图5是3DOM Ag/CeO2-ZrO2复合光催化剂的N2吸附-脱附等温线。
图6是3DOM Ag/CeO2-ZrO2复合光催化剂的XPS图。
图7是紫外光下直接光降解、P25、CeO2、ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2催化降解刚果红动力学结果图。
图8是可见光下直接光降解、P25、CeO2、ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2催化降解刚果红反应结果图。
图9是模拟日光下直接光降解、P25、CeO2、ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2催化降解刚果红反应结果图。
图10是P25、ZrO2、3DOM ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2在Na2S-Na2SO3溶液中光解水制氢结果图。
具体实施方式
减压填充法合成Ag掺杂3DOM CeO2-ZrO2复合光催化剂，称取购于天津科密欧化学试剂有限公司99.0%的Ce(NO3)3·6H2O，质量为Ce(NO3)3·6H2O，0.167±0.002 g，和购于天津市光复精细化工研究所99.8%的AgNO3，质量为0.023±0.001 g溶解于购于天津市光复精细化工研究所的99.7%的IPA中，体积为2 mL备用。将购于上海萨恩化学技术有限公司Mn~5800的P123，质量为0.050±0.005 g加入到体积为的15 mL IPA中并搅拌至完全溶解后滴加购于上海迈瑞尔化学技术有限公司80.0%的Zr(OC4H9)4，体积为1.5 mL，随后加入Ce(NO3)3与AgNO3溶液至形成Ag/CeO2-ZrO2溶胶，将PS模板(采用无乳化剂的乳化方法合成，并通过离心干燥获得PS胶晶模板)，质量为0.500±0.010 g置于Ag/CeO2-ZrO2溶胶中，搅拌一段时间后进行减压填充。将产物放入烘箱中至干燥，设定烘干温度60±2 ℃，干燥后所获产物使用天津泰斯特仪器有限公司的SX-2.5-12型箱式电阻炉中在600 ℃下煅烧7 h，得到三维有序大孔复合材料Ag/CeO2-ZrO2 (标记为3DOM Ag/CeO2-ZrO2)。
22复合光催化剂的结构及性能测定：
一、表面形貌和微观结构
3DOM Ag/CeO2-ZrO2样品的表面形貌和微观结构分析结果见图1—6。由图1可清楚地观察到，所合成的PS胶晶模板在三维空间内排列整齐有序，大小均一。由于在自组装过程中受到挤压，所以PS胶球呈现六边形形状。图2的SEM结果表明，样品在排列有序，呈开放通透的大孔结构，大孔排列整齐有序且为六边形形状，且由于PS胶晶模板为面心立方排列，所以能够从每个大孔处看到三个小孔。图3为样品3DOM Ag/CeO2-ZrO2的HR-TEM照片，从图中可以看到立方相Ag的(111)晶面，立方相CeO2的(111)晶面和四方相ZrO2的(011)晶面。图4为所制备的材料的XRD图，从图中可以看到，复合材料3DOM Ag/CeO2-ZrO2中存在Ag、CeO2和ZrO2的特征峰。图5为复合材料的N2吸附-脱附等温线，从图中可以明显的看到，由于具有较大的比表面积，三维有序大孔复合材料的等温线明显的向上移动。从图6的XPS图中也可以证明，在3DOM Ag/CeO2-ZrO2中Ce存在两种价态且Ag以单质的形式存在。
二、光催化性能测定
对所合成的3DOM Ag/CeO2-ZrO2的光催化活性进行了降解刚果红和光解水制氢的光催化实验。为了评价所合成的复合材料的光催化效果，选用市售P25、单质CeO2、单质ZrO2、Ag/CeO2-ZrO2及3DOM ZrO2作为对比实验。
、不同样品对紫外光降解刚果红速率的影响见图7所示。根据实验数据，按照公式- ln(C t /C 0 )=kt+b进行计算，其中，C t 为染料在t时刻的浓度(mg·L-1)，C 0 是染料初始浓度(mg·L-1)，k是速率常数(min-1)，b为截距。由图7可见，-ln(C t /C 0 )与反应时间t基本呈线性关系，这说明染料刚果红的降解遵循准一级反应动力学。经计算，直接光降解、P25、CeO2、ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2的紫外光光催化降解刚果红的表观反应速率常数分别为0.00053、0.00813、0.00652、0.00484、0.00902和0.01331 min-1。在可见光和模拟日光条件下降解刚果红结果见图8、图9，3DOM Ag/CeO2-ZrO2复合材料对刚果红的降解均呈现出最高的光催化活性，远超过市售P25。
2、光解水制氢P25、ZrO2、3DOM ZrO2、Ag/CeO2-ZrO2和3DOM Ag/CeO2-ZrO2不同样品在Na2S-Na2SO3溶液中产氢速率结果如图10所示。结果表明，3DOMAg/CeO2-ZrO2复合材料具有最好的产氢能力。
Claims (1)
1.一种Ag掺杂3DOM CeO2-ZrO2复合光催化剂的减压填充方法，其特征在于：称取P123，质量为0.050±0.005g，异丙醇，体积为17mL，PS，质量为0.500±0.010g，Zr(OC4H9)4，体积为1.5mL，Ce(NO3)3·6H2O，质量为0.167±0.002g，AgNO3，质量为0.023±0.001g；
Ce(NO3)3·6H2O与AgNO3溶解于2mL异丙醇中备用，将P123加入到异丙醇中并搅拌至完全溶解后滴加Zr(OC4H9)4，随后加入Ce(NO3)3与AgNO3溶液至形成Ag/CeO2-ZrO2溶胶，将PS模板置于Ag/CeO2-ZrO2溶胶中，搅拌一段时间后进行减压填充，将产物放入烘箱中至干燥，设定烘干温度60±2℃，干燥后所获产物在600℃下煅烧7h，得到三维有序大孔复合材料Ag/CeO2-ZrO2，标记为3DOM Ag/CeO2-ZrO2；
所述三维有序大孔复合材料Ag/CeO2-ZrO2中，Ag为立方相晶型，以单质形式存在；CeO2为立方相；ZrO2为四方相；
所述三维有序大孔复合材料Ag/CeO2-ZrO2用于降解刚果红和光解水制氢。
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| CN104607187A (zh) * | 2015-01-26 | 2015-05-13 | 北京工业大学 | 一种热稳定的贵金属掺杂型的三维有序大孔-介孔三效催化剂及制备方法和应用 |
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