CN110743541B - 铑掺杂钛酸锶反蛋白石材料及其制备方法与其在压电协同光催化去除有机污染物中的应用 - Google Patents
铑掺杂钛酸锶反蛋白石材料及其制备方法与其在压电协同光催化去除有机污染物中的应用 Download PDFInfo
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- CN110743541B CN110743541B CN201910960100.1A CN201910960100A CN110743541B CN 110743541 B CN110743541 B CN 110743541B CN 201910960100 A CN201910960100 A CN 201910960100A CN 110743541 B CN110743541 B CN 110743541B
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- rhodium
- strontium titanate
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000000463 material Substances 0.000 title claims abstract description 55
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 17
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 229920002223 polystyrene Polymers 0.000 claims abstract description 25
- 238000001354 calcination Methods 0.000 claims abstract description 22
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- 239000004038 photonic crystal Substances 0.000 claims abstract description 18
- 239000011521 glass Substances 0.000 claims abstract description 17
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- 239000000243 solution Substances 0.000 claims description 54
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 30
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- TYLYVJBCMQFRCB-UHFFFAOYSA-K trichlororhodium;trihydrate Chemical compound O.O.O.[Cl-].[Cl-].[Cl-].[Rh+3] TYLYVJBCMQFRCB-UHFFFAOYSA-K 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 11
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 abstract description 17
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 15
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 abstract description 14
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
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- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 150000003841 chloride salts Chemical class 0.000 description 1
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- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
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- 238000011067 equilibration Methods 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 description 1
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical group [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Abstract
本发明公开了一种铑掺杂钛酸锶反蛋白石材料及其制备方法与其在去除有机污染物中的应用；通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；将三维有序的光子晶体蛋白石模板浸入含有铑源、钛源、锶源的溶液中，再通过煅烧制备铑掺杂钛酸锶反蛋白石材料；将铑掺杂钛酸锶反蛋白石材料加入含有污染物的水中，然后光照和/或超声处理，完成水中污染物的去除。本发明的三维有序大孔铑掺杂钛酸锶反蛋白石材料能够被应用在光催化领域，在外力作用下，材料自发极化所形成的内置电场能够有效分离光致载流子，从而能够增强光催化性能，提高光催化效率。
Description
技术领域
本发明属于无机纳米材料及压电协同光催化技术领域，具体涉及一种对可见光响应的三维有序大孔铑掺杂钛酸锶反蛋白石材料的制备方法及其在压电协同可见光催化降解水体中有机污染物的应用。
背景技术
随着工业化快速发展，污水排放量迅速增加，水污染问题越来越严峻。传统的废水处理方法通常具有能耗大，不能兼容环境的特点，因此需要寻求高效绿色的污水处理方法以治理环境。最近，已报道了许多安全有效、绿色环保的修复方法来消除水生环境中的有机污染物，包括物理吸附、化学氧化、生物降解等。在这些方法中，光催化降解因具有环境友好性高，效率高，成本相对较低，操作条件简便等优点，被认为是最有潜力的选择。
然而，一些单组分光催化剂在应用中存在着一些缺陷，例如较高的光生电子-空穴复合率，这导致了其较低的光量子效率和较低的光催化性能。钛酸锶（SrTiO3）是一种钙钛矿型光催化材料，具有高稳定性、耐酸碱性好、光照后不发生阳极光腐蚀、来源丰富、安全无毒、低成本等优点，同时它也拥有优异的铁电、压电、光电等性能，因而被广泛研究。然而，钛酸锶的宽带隙仅能吸收太阳光中的紫外光，这极大地限制了它的实际应用。
发明内容
本发明的目的是提供一种对可见光响应的三维有序大孔反蛋白石材料，并且用相对廉价的过渡金属铑的氯化盐代替金、铂、钯等贵金属对钛酸锶进行微量的掺杂改性，解决了高昂的成本问题；同时本发明公开的材料能够通过压电协同光催化作用快速高效降解水体中的有机污染物。本发明的三维有序大孔铑掺杂钛酸锶反蛋白石材料能够被应用在光催化领域，在超声等外力作用下，材料自发极化所形成的内置电场能够有效分离光致载流子，从而能够增强光催化性能，提高光催化效率。
为达到上述目的，本发明具体技术方案如下：
钛酸锶反蛋白石材料，其制备方法包括以下步骤：
（1）通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；
（2）将三维有序的光子晶体蛋白石模板浸入含有钛源、锶源的溶液中，再通过煅烧制备钛酸锶反蛋白石材料。
铑掺杂钛酸锶反蛋白石材料，其制备方法包括以下步骤：
（1）通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；
（2）将三维有序的光子晶体蛋白石模板浸入含有铑源、钛源、锶源的溶液中，再通过煅烧制备铑掺杂钛酸锶反蛋白石材料。
一种催化去除水中污染物的方法，包括以下步骤：
（1）通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；
（2）将三维有序的光子晶体蛋白石模板浸入含有铑源、钛源、锶源的溶液中，再通过煅烧制备铑掺杂钛酸锶反蛋白石材料；或将三维有序的光子晶体蛋白石模板浸入含有钛源、锶源的溶液中，再通过煅烧制备钛酸锶反蛋白石材料；
（3）将铑掺杂钛酸锶反蛋白石材料或者钛酸锶反蛋白石材料加入含有污染物的水中，然后光照和/或超声处理，完成水中污染物的去除。
本发明中，步骤（1）中，将单分散聚苯乙烯微球乳液铺在FTO玻璃具有导电性的一面上，恒温处理，制备三维有序的光子晶体蛋白石模板；优选的，FTO玻璃依次用丙酮、乙醇和去离子水超声清洗；单分散聚苯乙烯微球乳液的浓度为0.125 wt%；进一步优选的，单分散的聚苯乙烯微球的粒径为250～300nm，优选280 nm；恒温处理的温度为40～50℃，时间为45～75小时。
本发明中，步骤（2）中，煅烧前经过干燥，优选干燥温度为50～70 ℃，煅烧温度为400～650 ℃，升温速率为1～2 ℃/min，时间为1.5～2.5小时；铑源为氯化铑或硝酸铑，锶源为硝酸锶或醋酸锶，钛源为钛酸四正丁酯或钛酸四异丙酯；含有铑源、钛源、锶源的溶液中或者含有钛源、锶源的溶液中，溶剂为水，优选的，含有铑源、钛源、锶源的溶液或者含有钛源、锶源的溶液，还含有乙酸、柠檬酸。优选的，铑掺杂钛酸锶反蛋白石材料中，铑的掺杂量为锶摩尔量的0~1%。
本发明中，步骤（3）中，污染物为双酚A；光照处理为300 W氙灯光照处理，超声处理的功率为100~150 W；优选光照同时通过施加超声提供外加机械振动以激发材料内部的压电效应，在外力作用下，材料自发极化所形成的内置电场能够有效分离光致载流子，从而能够增强光催化性能，提高光催化效率。
本发明铑掺杂钛酸锶反蛋白石材料中，钙钛矿钛酸锶是最重要的n型半导体之一，具有大量的光催化位点，优异的耐光腐蚀性，热稳定性以及作为金属负载主体的良好结构稳定性并且成本低廉；反蛋白石材料的周期性结构表现出明显的慢光子效应，它可以禁止某些波长的光在材料中传播并产生阻带反射，并且慢光子效应也可以增加光的路径长度，增强光子-物质相互作用进一步提高半导体的光能转换效率。
本发明公开了上述钛酸锶反蛋白石材料或者铑掺杂钛酸锶反蛋白石材料在去除有机污染物中的应用；优选的有机污染物为双酚A。
由于上述技术方案的运用，本发明与现有技术相比具有下列优点：
1. 本发明的ABO3型钙钛矿结构，掺杂剂可以占据其A和B位置，同时掺杂后还能够保持稳定的钙钛矿结构，并且掺杂剂的选择具有极大的灵活性，尤其是本发明铑掺杂钛酸锶反蛋白石材料光响应范围从紫外光区移动到可见光区并且能有效地改善钛酸锶在可见光区的光催化活性，解决了现有许多过渡金属元素掺入钛酸锶晶格，但不能够将钛酸锶光响应范围从紫外光区移动到可见光区的缺陷。
2. 本发明公开的钛酸锶反蛋白石材料是在FTO基底上自组装聚苯乙烯微球，然后制备掺杂钛酸锶前驱体，并通过毛细管力将前驱体填充到蛋白石模板的缝隙中，通过煅烧的方法将模板去除，从而得到三维孔洞结构。铑掺杂钛酸锶反蛋白石的周期性结构可以增加光的路径长度，增强光子-物质相互作用，进一步增强光的吸收，利用更多的光子，从而进一步提高半导体的光能转换效率，增强材料的光催化性能。同时，其三维有序多孔结构比普通纳米颗粒材料具有更大的比表面积，有利于暴露催化剂的活性位，对光在其内部的传播有多重散射作用。
3. 本发明公开的铑掺杂钛酸锶反蛋白石也是一种压电材料，当外力作用时，由于其自发极化，在钛酸锶内部形成电场，可以有效地分离电子和空穴，实现在外力作用下对有机污染物的光催化分解，提高光催化活性。同时它又不具有传统压电材料锆钛酸铅（PZT）所具有的毒性，且成本低廉，有利于进一步的推广应用。
附图说明
图1为实施例三的钛酸锶反蛋白石（SrTiO3 IO）的扫描电镜图；
图2为实施例四的铑掺杂钛酸锶反蛋白石（Rh-SrTiO3 IO）的扫描电镜图；
图3为实施例四的铑掺杂钛酸锶反蛋白石（Rh-SrTiO3 IO）的透射电镜图；
图4为实施例四的铑掺杂钛酸锶反蛋白石（Rh-SrTiO3 IO）的紫外可见吸收光谱图；
图5为实施例六的钛酸锶反蛋白石（SrTiO3 IO）和铑掺杂钛酸锶反蛋白石（Rh-SrTiO3 IO）降解双酚A的效果图。
具体实施方式
本发明通过掺杂过渡金属元素和微观形貌调控对钛酸锶纳米材料进行改性，采用模板煅烧法制备得到铑掺杂钛酸锶反蛋白石（Rh-SrTiO3 IO），以达到调节钛酸锶带隙的目的，使其对可见光产生响应；同时能够利用反蛋白石独特的三维有序大孔的结构特点，提高光的吸收、暴露更多的活性位点，增强光催化性能。此外，本发明的三维有序大孔铑掺杂钛酸锶反蛋白石材料是一种良好的压电材料，本发明在光催化过程中，对其施加外部机械力，产生内置极化电场，使得光生电子空穴进一步分离，从而进一步提高光催化性能，实现对水体中有机污染物的高效去除。
本发明钛酸锶反蛋白石材料的制备方法如下：
（1）通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；
（2）将三维有序的光子晶体蛋白石模板浸入含有钛源、锶源的溶液中，再通过煅烧制备钛酸锶反蛋白石材料。
铑掺杂钛酸锶反蛋白石材料的制备方法如下：
（1）通过垂直沉积法将单分散的聚苯乙烯微球自组装在FTO玻璃具有导电性的一面，制备三维有序的光子晶体蛋白石模板；
（2）将三维有序的光子晶体蛋白石模板浸入含有铑源、钛源、锶源的溶液中，再通过煅烧制备铑掺杂钛酸锶反蛋白石材料。
优选的，含有铑源、钛源、锶源的溶液由乙酸、柠檬酸、水、铑源、钛源、锶源组成；含有钛源、锶源的溶液由乙酸、柠檬酸、水、钛源、锶源组成。
下面结合实施例对本发明作进一步描述。
实施例一
光子晶体蛋白石模板的制备：通过垂直沉积法制备，首先将FTO玻璃依次用丙酮、乙醇和去离子水超声20 min；再将冻干的280 nm聚苯乙烯微球粉末分散到去离子水中，得到0.125 wt%单分散聚苯乙烯微球乳液。然后量取1 ml的浓度为0.125 wt%的单分散聚苯乙烯微球乳液于称量瓶中，把超声干净的FTO玻璃具有导电性的一面朝上垂直放入到称量瓶中，将称量瓶适当倾斜，使液面恰好接触到FTO玻璃基板边缘（即将单分散聚苯乙烯微球乳液铺在FTO玻璃具有导电性的一面上），再放入到45℃的电热恒温培养箱中，保持两天（48小时），即可制得三维有序的光子晶体模板，用于实施例二至实施例五。
实施例二
钛酸锶反蛋白石的制备：首先，将0.01 mol钛酸四丁酯与10 mL乙酸混合，然后在连续搅拌下将10 mL去离子水滴加到该溶液中。之后，在上述溶液中滴加10 mL 1M Sr(NO3)2。最后，再加入10 mL 2M柠檬酸溶液。将所得溶液在室温下再搅拌30分钟，得到澄清溶液，记为溶液A。将制备好的聚苯乙烯蛋白石模板浸泡在溶液A中，然后置于60 ℃烘箱干燥烘干，再将干燥好的前驱体模板使用管式炉在空气中煅烧2 h，煅烧温度为650 ℃，升温速率2 ℃/min（室温升至650℃），自然冷却得到钛酸锶反蛋白石薄膜光催化剂（SrTiO3 IO）。从附图1中可以看出，钛酸锶反蛋白石呈三维有序大孔结构，孔径均一，排列规则。
实施例三
0.3 mol%铑掺杂钛酸锶反蛋白石的制备：首先，将钛酸四丁酯与10 mL乙酸混合，然后在连续搅拌下将10 mL去离子水滴加到该溶液中。之后，在上述溶液中滴加10 mL 1 M硝酸锶和三水合三氯化铑的混合溶液（钛酸四丁酯与三水合三氯化铑的摩尔数之和为硝酸锶的摩尔数），三水合三氯化铑的摩尔数为硝酸锶摩尔数的0.3 %。最后，再加入10 mL 2 M柠檬酸溶液。将所得溶液在室温下再搅拌30分钟，得到澄清溶液，记为溶液A。将制备好的聚苯乙烯蛋白石模板浸泡在溶液A中，然后置于60 ℃烘箱干燥烘干，将干燥好的前驱体模板使用管式炉在空气中煅烧2 h，煅烧温度为650 ℃，升温速率2 ℃/min（室温升至650℃），自然冷却得到铑掺杂钛酸锶反蛋白石薄膜光催化剂（0.3 mol% Rh-SrTiO3 IO）。
实施例四
0.5 mol%铑掺杂钛酸锶反蛋白石的制备：首先，将钛酸四丁酯与10 mL乙酸混合，然后在连续搅拌下将10 mL去离子水滴加到该溶液中。之后，在上述溶液中滴加10 mL 1 M硝酸锶和三水合三氯化铑的混合溶液（钛酸四丁酯与三水合三氯化铑的摩尔数之和为硝酸锶的摩尔数），三水合三氯化铑的摩尔数为硝酸锶摩尔数的0.5 %。最后，再加入10 mL 2 M柠檬酸溶液。将所得溶液在室温下再搅拌30分钟，得到澄清溶液，记为溶液A。将制备好的聚苯乙烯蛋白石模板浸泡在溶液A中，然后置于60 ℃烘箱干燥烘干，将干燥好的前驱体模板使用管式炉在空气中煅烧2 h，煅烧温度为650 ℃，升温速率2 ℃/min（室温升至650℃），自然冷却得到铑掺杂钛酸锶反蛋白石薄膜光催化剂（0.5 mol% Rh-SrTiO3 IO）。从附图2中可以看出，0.5 mol%铑掺杂钛酸锶反蛋白石依然保持稳定的骨架，孔洞均匀，结构规则。
实施例五
1.0 mol%铑掺杂钛酸锶反蛋白石的制备：首先，将钛酸四丁酯与10 mL乙酸混合，然后在连续搅拌下将10 mL去离子水滴加到该溶液中。之后，在上述溶液中滴加10 mL 1 M硝酸锶和三水合三氯化铑的混合溶液（钛酸四丁酯与三水合三氯化铑的摩尔数之和为硝酸锶的摩尔数），三水合三氯化铑的摩尔数为硝酸锶摩尔数的1.0 %。最后，再加入10 mL 2 M柠檬酸溶液。将所得溶液在室温下再搅拌30分钟，得到澄清溶液，记为溶液A。将制备好的聚苯乙烯蛋白石模板浸泡在溶液A中，然后置于60 ℃烘箱干燥，将干燥好的前驱体模板使用管式炉在空气中煅烧2 h，煅烧温度为650 ℃，升温速率2 ℃/min（室温升至650℃），自然冷却得到铑掺杂钛酸锶反蛋白石薄膜光催化剂（1.0 mol% Rh-SrTiO3 IO）。
对比例
铑掺杂钛酸锶纳米颗粒的制备：通过水热法合成，首先将钛酸四丁酯溶解于20 mL乙二醇中形成澄清溶液，然后在磁力搅拌下向其中逐滴加入20 mL 0.5 M硝酸锶和三水合三氯化铑的混合水溶液以及10 mL 5 M氢氧化钠溶液（其中硝酸锶、钛酸四丁酯、三水合三氯化铑的摩尔数比为1:0.995:0.005）。搅拌30分钟后，将混合物加入100mL高压反应釜中，在200℃下反应24小时。反应结束后，用去离子水和无水乙醇洗涤产物多次，直到pH达到7。然后将产物在70℃下干燥过夜，获得铑掺杂钛酸锶纳米颗粒（Rh-SrTiO3 NPs）。
实施例六
0.5 mol% Rh-SrTiO3 IO对双酚A的压电光催化降解实验：称取6 mg上述实施例四中所得光催化剂0.5 mol% Rh-SrTiO3 IO，置于10mL 浓度为10 mg/L 的双酚A水溶液。避光搅拌一小时，达到吸附-解吸平衡。平衡后，将装有双酚A水溶液的试管斜置于超声清洁器中，使用300 W氙灯照射催化剂并打开超声清洁器，功率调至150 W，每15分钟取样1 mL，使用高效液相色谱记录保留时间，记录此保留时间
对应的液相出峰面积，得到相应水样中双酚A的浓度。附图5为双酚A的残留率与时间的关系曲线图。从图中可以看出，在加入0.5 mol% Rh-SrTiO3 IO光催化剂，并且在同时施加光照和超声的条件下，光照30 min后，水溶液中双酚A被完全去除（残留0%）。同样的方法测试其他实施例的催化剂材料，光照30 min后，水溶液中双酚A的残留率分别为，实施例二15%、实施例三7%、实施例五9%、对比例43%。
将实施例四中的铑掺杂更换为同摩尔量的钌掺杂，同样的制备方法得到的0.5mol% Ru-SrTiO3 IO，经过上述同样的双酚A的压电协同光催化降解实验，光照30 min后，水溶液中双酚A残留13%。
将实施例一的聚苯乙烯微球的粒径更换为420 nm，其余方法一样，得到0.5 mol%Rh-SrTiO3 IO经过上述同样的双酚A的压电协同光催化降解实验，光照30 min后，水溶液中双酚A残留6%，说明模板的孔径大小对反蛋白石的慢光子效应（对光的吸收利用率）有一定影响，进而影响材料的光催化性能。
将实施例六中的超声更换为磁力搅拌（200rpm），其余方法一样，将0.5 mol% Rh-SrTiO3 IO经过上述同样的双酚A的光催化降解实验，光照30 min后，水溶液中双酚A残留52%，由此说明超声振动引起的机械应力在光催化降解双酚A实验中起到了较大的作用。
本发明公开了一种铑掺杂钛酸锶反蛋白石材料的制备方法及其在压电协同光催化去除水体中有机污染物（双酚A）的应用。首先通过无皂乳液聚合制备聚苯乙烯，使用垂直沉积法得到聚苯乙烯蛋白石，通过一步煅烧法得到一种铑掺杂钛酸锶反蛋白石新型无机纳米材料。本发明制备的铑掺杂钛酸锶反蛋白石，含d轨道电子的过渡金属元素Rh3+可被掺杂进钛酸锶的晶格，有效降低钛酸锶的带隙使其具有可见光响应，解决了钛酸锶仅对紫外光产生响应导致其应用得到限制的问题。同时，本发明制备的钛酸锶反蛋白石是一种三维周期性孔洞结构，且具有慢光子效应，使其相对于普通的多孔材料，在光催化方面表现出更好的催化性能。此外，钛酸锶还是一种良好的压电材料，在光催化过程中，可对其施加外部机械压力，产生内置极化电场，使得光生电子空穴进一步得到分离。因此，掺杂后的低带隙加上自身压电性质使得钛酸锶能够充分利用慢光子效应和振动能量催化降解有机污染物，无需将其与其他材料耦合或利用外部偏压，降低使用成本。
Claims (2)
1.一种铑掺杂钛酸锶反蛋白石材料在去除双酚A中的应用，其特征在于，将铑掺杂钛酸锶反蛋白石材料加入含有污染物的水中，然后光照和超声处理，完成水中污染物的去除；所述铑掺杂钛酸锶反蛋白石材料制备方法包括以下步骤：
（1）将FTO玻璃依次用丙酮、乙醇和去离子水超声20 min；再将冻干的280 nm聚苯乙烯微球粉末分散到去离子水中，得到0.125 wt%单分散聚苯乙烯微球乳液；然后量取1 ml的浓度为0.125 wt%的单分散聚苯乙烯微球乳液于称量瓶中，把超声干净的FTO玻璃具有导电性的一面朝上垂直放入到称量瓶中，将单分散聚苯乙烯微球乳液铺在FTO玻璃具有导电性的一面上，再放入到45℃的电热恒温培养箱中，保持两天，制备三维有序的光子晶体蛋白石模板；
（2）将钛酸四丁酯与10 mL乙酸混合，然后在连续搅拌下将10 mL去离子水滴加到该溶液中；之后，在上述溶液中滴加10 mL 1 M硝酸锶和三水合三氯化铑的混合溶液，三水合三氯化铑的摩尔数为硝酸锶摩尔数的0.5 %；最后，再加入10 mL 2 M柠檬酸溶液；将所得溶液在室温下再搅拌30分钟，得到澄清溶液，记为溶液A；将制备好的三维有序的光子晶体蛋白石模板浸泡在溶液A中，然后置于60 ℃烘箱干燥烘干，将干燥好的前驱体模板使用管式炉在空气中煅烧2 h，煅烧温度为650 ℃，升温速率2 ℃/min，自然冷却得到铑掺杂钛酸锶反蛋白石材料；钛酸四丁酯与三水合三氯化铑的摩尔数之和为硝酸锶的摩尔数。
2.根据权利要求1所述的应用，其特征在于，光照处理为300 W氙灯光照处理，超声处理的功率为100~150 W。
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