CN108620128B - 一种可见光响应的FePc/BiOBr复合光催化剂的制备方法 - Google Patents
一种可见光响应的FePc/BiOBr复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及到一种可见光响应的FePc/BiOBr复合光催化剂的制备方法，包括下述步骤：(1)称取15～20mmol四甲基溴化铵、0.1～1.0mmol的酞菁铁加入到25～35ml三乙二醇中，在超声波清洗器中300～800W下超声0.5～1.5h得到酞菁铁、四甲基溴化铵混合溶液；(2)称取6～12mmol醋酸铋加入到装有25～35ml三乙二醇的烧杯中，在200～500rpm下搅拌1～3h后得到醋酸铋醇溶液；(3)将两种溶液混合搅拌后用聚四氟乙烯内胆盛放，并放置于不锈钢高压反应釜中于150～190℃下反应2～8h；产物抽滤、洗涤后，置于40～60℃真空干燥箱内真空干燥12～48h，得到FePc/BiOBr复合光催化剂。
Description
技术领域
本发明涉及到光催化剂技术领域，尤其涉及一种对可见光响应的催化剂的制备方法。
背景技术
传统的光催化剂TiO2具有很好的化学稳定性，优良的光催化活性并能氧化空气和水中的污染物，但TiO2的宽能带带隙(3.2e V)只允许它吸收紫外线(<387nm)，这意味着太阳光谱中，只有3％-5％的能量是可以利用的。因此限制了它在很多领域中的应用。相较于传统的光催化剂，可见光光催化剂可以对可见光响应，并可以利用太阳光对污染物进行催化降解，节约成本。可见光响应的光催化报道较少
发明内容
本发明所要解决的技术问题是针对现有技术的现状提供一种成本低、稳定性好能够在可见光光源的照射下光催化降解有机染料废水的催化剂的制备方法。
本发明解决上述技术问题所采用的技术方案为：该可见光响应的FePc/BiOBr复合光催化剂的制备方法，其特征在于包括下述步骤：
(1)分别称取15～20mmol四甲基溴化铵、0.1～1.0mmol的酞菁铁加入到25～35ml三乙二醇中，在超声波清洗器中300～800W下超声0.5～1.5h得到酞菁铁、四甲基溴化铵混合溶液；
(2)称取6～12mmol醋酸铋加入到装有25～35ml三乙二醇的烧杯中，在200～500rpm下搅拌1～3h后得到醋酸铋醇溶液；
(3)将步骤(1)所得的混合溶液加入到步骤(2)所得的醋酸铋醇溶液中，200～500rpm下搅拌0.5～1.5h后加入到聚四氟乙烯内胆中，填充体积为60％～80％，将装好反应溶液的内胆放置于不锈钢高压反应釜中，再将密封好的反应釜置于烘箱内150～190℃下反应2～8h；反应后将反应釜取出，室温下静置自然冷却至室温，打开反应釜，用滤纸将内胆中沉淀下来的固体通过抽滤分离出来，所收集的沉淀物用超纯水清洗三次，乙醇清洗一次。最后把洗净的材料置于40～60℃真空干燥箱内真空干燥12～48h，得到FePc/BiOBr复合光催化剂。
上述方案所制备的催化剂使用后的回收方法，其特征在于包括下述步骤：
将使用后的催化剂在600～1000rpm下离心，然后用清水洗涤三次，在20～60℃下真空干燥箱内真空干燥10～15小时后，即得到回收的催化剂。
与现有技术相比，本发明所提供了一种新型FePc/BiOBr复合光催化剂，该催化剂制备方法简单可行，该复合光催化剂在可见光照射下能在短时间内快速降解酸性红B废水，且效率高、稳定性好可重复利用。
附图说明
图1为本发明实施例中FePc/BiOBr复合光催化剂的扫描电镜照片；
图2为本发明实施例FePc/BiOBr催化剂在可见光下降解酸性红B；
图3为本发明实施例中回收的FePc/BiOBr催化剂多次循环利用的光催化性能。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
1、制备FePc/BiOBr复合光催化剂：
分别称取16mmol四甲基溴化铵、0.15mmol的酞菁铁加入到盛有30ml三乙二醇的烧杯中，在超声波清洗器中400W下超声1h得到酞菁铁、四甲基溴化铵混合溶液。
称取6.5mmol醋酸铋加入到装有30ml三乙二醇的烧杯中，在400rpm下搅拌1.5h后得到醋酸铋醇溶液。
将酞菁铁、四甲基溴化铵混合溶液加入到醋酸铋醇溶液中400rpm下搅拌1h后，加入到聚四氟乙烯内胆中，填充体积为70％。将装好反应溶液的内胆放置于不锈钢高压反应釜中，再将密封好的反应釜置于烘箱内150℃下反应2h，反应后将反应釜取出，室温下静置自然冷却至室温。
聚四氟乙烯内胆是指用聚四氟乙烯材质制备的容器。
打开反应釜，用滤纸将内胆中沉淀下来的固体通过抽滤分离出来，所收集的沉淀物用超纯水清洗三次。最后把洗净的材料置于40℃真空干燥箱内真空干燥12h，得到0.13g的FePc/BiOBr复合光催化剂。
电镜扫描
将实施例1的FePc/BiOBr复合光催化剂在日立高新扫描电子显微镜SEM SU3500中进行分析测试，其中各参数设置如下：加速电压：20kV，放大倍率：25～200.000，分辨率：3.5nm，真空度：6×l0-6Pa。
图1为FePc/BiOBr复合光催化剂的SEM图。
从图1可以看出：BiOBr以片层结构堆积在一起；FePc为颗粒状，嵌在BiOBr的片层结构之间。
催化活性测试
以酸性红B作为目标降解物，采用120W的LED光源(波长大于400nm)为可见光源，研究合成的FePc/BiOBr复合光催化剂在可见光下的光催化活性。具体实验过程为：
将0.05g的FePc/BiOB粉体加入到盛有150ml浓度为15mg/L的酸性红B溶液的石英反应器中，将反应器在暗室避光搅拌30min以达到吸附-脱附平衡，打开光源，用120W、波长大于400nm的LED光源照射；每隔15min取一次样，离心，取上清液。
采用可见光分光光度计测定酸性红B溶液的吸光度，以酸性红B的脱色率(降解过程中t时刻浓度/初始浓度)表征降解的程度。如图2所示。
由图2可以看出，本实施例制备的催化剂在60min内可以使酸性红B降解率达到97％。
回收催化剂催化活性测试
将催化活性测试实验使用过的催化剂在800rpm离心，用清水洗涤三次，在40℃真空干燥箱内真空干燥12h，重复上述光催化活性实验。
然后对再次使用过的催化剂进行回收，测试其光催化活性。
重复上述实验六次，测试结果如图3所示。
从图3中可以看出回收的催化剂稳定性好，第5次循环使用可以在60min内使酸性红B降解率达到90％。
Claims (1)
1.一种可见光响应的FePc/BiOBr复合光催化剂的制备方法，其特征在于包括下述步骤：
(1)分别称取16mmol四甲基溴化铵、0.15mmol的酞菁铁加入到盛有30ml三乙二醇的烧杯中，在超声波清洗器中400W下超声1h得到酞菁铁、四甲基溴化铵混合溶液；
(2)称取6.5mmol醋酸铋加入到装有30ml三乙二醇的烧杯中，在400rpm下搅拌1.5h后得到醋酸铋醇溶液；
(3)将酞菁铁、四甲基溴化铵混合溶液加入到醋酸铋醇溶液中400rpm下搅拌1h后，加入到聚四氟乙烯内胆中，填充体积为70％；将装好反应溶液的内胆放置于不锈钢高压反应釜中，再将密封好的反应釜置于烘箱内150℃下反应2h，反应后将反应釜取出，室温下静置自然冷却至室温；
(4)打开反应釜，用滤纸将内胆中沉淀下来的固体通过抽滤分离出来，所收集的沉淀物用超纯水清洗三次；最后把洗净的材料置于40℃真空干燥箱内真空干燥12h，得到0.13g的FePc/BiOBr复合光催化剂。
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