CN108097234A - 一种可见光响应型光催化剂及其制备方法 - Google Patents
一种可见光响应型光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种可见光响应型光催化剂及其制备方法，所述光催化剂其化学式为:Ce‑Sr2Bi2O5，Ce/Bi为0.5%～20%；以氧化铋和碳酸锶为原料、氧化铈为掺杂剂，通过固相法制备而成。本发明不仅能在紫外线范围,而且可在可见光范围内对液相中的有害化学物质进行分解处理,对含复杂苯环结构的亚甲基蓝溶液的降解率比Sr2Bi2O5有显著提高；具有制备工艺简单易操作、生产效率高、催化活性高、催化效率高等优点，原料易得，重现性高，适用于工业生产。
Description
技术领域
本发明涉及一种无机材料Ce-Sr2Bi2O5及其制备方法，属于无机光催化材料技术领域。
背景技术
环境污染问题制约着社会的发展与进步，废水处理和空气净化备受关注。现在光催化技术已经在废水处理、气体净化、杀菌、防污、自洁材料、染料敏化太阳能电池、化妆品、气体传感器等许多领域有着广泛的应用。目前，国内外研究最多的半导体光催化材料主要是金属氧化物和硫化物，如Ti02，W03，ZnO，Fe203，CdS等。活性较高的TiO2和 ZnO等宽禁带半导体材料，仅能被紫外光所激发，如纳米TiO2光催化材料的带隙有3.2eV，对应的激活波长为380nm，即太阳光的紫外部分。而紫外光能量在太阳光中所占比例不到5%即光利用率低，而且就环境净化而言，对于没有紫外光的室内的应用也将受到限制。可见光催化材料能有效利用可见光区的太阳光，如CdS（2.5eV），Fe2O3(2.2e V),和 Cu2O(2.0e V)等氧化物（硫化物）窄带半导体，都能够被可见光激发而进行光催化分解水或降解有机污染物，且其结构简单，制备容易。但诸多研究证明，许多窄带半导体本身在紫外－可见光照射下，往往表现出不稳定性，即产生光蚀现象，如CdS 在水相悬浮光催化体系中，会发生如下的反应：2hvb++CdS = Cd2++S(hvb+为价带空穴)。因此，如何提高光催化剂的光催化活性和稳定性以及拓宽光吸收范围是当今的研究热点。
目前人们研究发现具有6s2电子结构的Bi3+离子由于价带能级较为分散，且含Bi3+氧化物半导体禁带宽度较窄又具有层状结构，十分利于光生电子与空穴的产生和快速迁移，是很好的控制半导体价带的元素。依此研究人员制备出可见光响应型高催化活性的铋酸盐光催化剂。如：K.Obata等（Preparation and characterization of SrO-Bi2O3complex oxide,Funct.Mater.Lett.5 (2012),260015-1.）以Sr(NO3)2和Bi(NO3)3·5H2O为原料通过液相法制备出Sr2Bi2O5光催化剂，但需要有机酸做络合剂，用氨水调节PH值，反应不宜控制，可见光光降解性能差；赵伟等（CN101933525）通过焙烧原位还原法，在Sr3BiO5.4表面得到了纳米级的Cu2O-CuO氧化物，该纳米Cu2O-CuO/Sr3BiO5.4复合金属氧化物具有可见光催化性能，然而制备过程比较复杂，复合物不易生成。
发明内容
本发明针对现有光催化剂存在的问题，提供一种具有制备工艺简单、催化活性高、对光源的利用率高、催化效率高、成本低等优点可见光响应型光催化剂。
为了实现以上目的，本发明采用Ce-Sr2Bi2O5作为可见光响应型催化剂，在可见光的照射下，对亚甲基蓝溶液具有很好的降解效果。
本发明的可见光响应型催化剂Ce-Sr2Bi2O5的制备方法，包括以下步骤：
(1)按照比例称取一定量的氧化铋和碳酸锶于球磨罐里，加入氧化铈；
(2)向上述球罐里加入适量去离子水和球磨玛瑙球；
(3)将上述球罐置于行星球磨机上进行球磨，在一定转速下球磨一段时间后得到的浆料进行干燥；
(4)干燥后的物料研磨过筛，然后置于马弗炉里进行焙烧，反应一段时间后自然降温，待其冷却后研磨过筛得到初始样品。
(5)将上样品置于马弗炉里进行焙烧，保温一段时间后自然降温，待其冷却后研磨过筛可得到所述可见光响应型光催化剂。
步骤（1）中氧化铋和碳酸锶的物质的量的比例为1：2，氧化铈与氧化铋物质的量的比例为0.01～0.4。
步骤（2）中玛瑙球与物料比为1～3:1，加去离子水淹没物料且体积为球罐容积的60%～90%。
步骤（3）中转速为200～400r/min，球磨时间为1～3小时。
步骤（4）中焙烧温度为600℃～900℃，保温时间为4h～8h，筛网目数为200～400目。
步骤（5）中焙烧温度为600℃～900℃，保温时间为4h～20h。
与现有技术相比，本发明的优点及有益效果为：1）本发明的制备工艺简单易操作，反应条件温和，能源消耗低，分段反应避免煅烧过程中化学计量容易发生改变生成第二相的问题，与传统的水热法制备工艺相比有省时省力、安全易操作、产率高等优点。2）本发明制备的光催化剂催化活性高 ,可见光下2小时对亚甲基蓝的降解率达到80%以上。3个小时能实现基本完全降解。3）本发明具有原料来源广泛易获得、成本低廉、制备工艺简单、生产效率高、能耗低、反应条件易控、催化活性高、催化效率高等优点，在可见光辐照下能高效催化降解废水有机污染物，具有很好的经济效益、社会效益和生态效益，更适用于工业生产。
附图说明
图1为本发明实施例2光催化剂的紫外-可见漫反射波谱图。
图2为本发明实施例1、2、3、4、5和对比例3、7光催化剂对亚甲基蓝溶液降解效果图。。
图3为本发明实施例1、2、3、4、5、6的光催化剂的XRD图谱。
具体实施方式
本发明不局限于下述实施例。
实施例1
称取2.9526g（20mmol）的碳酸锶和4.6596g（10mmol）的氧化铋球磨罐里，加入0.0344g（0.2mmol）氧化铈；向上述球罐里加入适量去离子水和球磨玛瑙球；将上述球罐置于行星球磨机上进行球磨，在300r/min下球磨3h后得到的浆料然后进行干燥；干燥后的物料研磨过筛，然后置于马弗炉里进行焙烧，750℃保温6h后自然降温，待其冷却后研磨过筛得到初始样品。将上样品置于马弗炉里进行焙烧，750℃保温12h后自然降温，待其冷却后研磨过筛可得到所述可见光响应型光催化剂。
实施例2～实施例6
采用与实施例1相同的方法，与之不同的是氧化铈分别为0.0688g（0.4mmol）、0.1377g（0.8mmol）、0.2065g（1.2mmol）、0.2754g（1.6mmol）、0.3442g（2mmol）。
对比例1
固相法制备Sr2Bi2O5：称取5.905g 碳酸锶和9.319g氧化铋于球磨罐里，然后加入适量去离子水和玛瑙球，将上述球罐置于行星球磨机上进行球磨，在300r/min下球磨3h后得到的浆料；把浆料放置干燥箱里干燥12小时，干燥后的物料研磨过筛，然后置于马弗炉里进行焙烧，500℃保温6h后自然降温，待其冷却后研磨过筛得到初始样品。将上样品置于马弗炉里进行焙烧，500℃保温12h后自然降温，待其冷却后研磨过筛可得到所述的固相法制备的可见光响应型光催化剂。
对比例2～对比例6
采用与对比例1相同的方法，与之不同的是热处理分别为600℃、700℃、750℃、800℃、850℃。
对比例7
液相法制备Sr2Bi2O5：称取15.280g（31.5mmol）的五水硝酸铋和6.349g（30mmol）的硝酸锶于烧杯里，加入120mL去离子水，室温下搅拌30min混合均匀，得溶液A；向溶液A中加入8.767g（30mmol）乙二胺四乙酸和6.616g（31.5mmol）柠檬酸，滴加氨水调节PH=8室温下搅拌30min制备成乳浊液；将乳浊液转置120℃烘箱里干燥12小时后得到前驱体；将前驱体转置马弗炉里，升温速度为10℃/min，700℃保温6小时后随炉壁冷却研磨过筛即可得到所述的可见光响应型Sr2Bi2O5光催化剂。
催化剂的光催化试验：将各实施例和对比例制备的光催化剂分别称取1g，放入具有1L亚甲基蓝模拟水样的烧杯里且亚甲基蓝溶液的浓度为8mg/L，以150W金卤灯作为光催化实验的光源，用滤光片（λ>400nm）截取可见光。在转速为500r/min下搅拌，先在黑暗条件下搅拌一个小时达到光催化剂与亚甲基蓝溶液的吸附平衡，然后打开金卤灯进行光照并同时打开循环水冷却装置以避免温度影响光催化实验，每隔一段时间取样，离心后用紫外可见光分光光度计测上清液的吸光度，计算降解率，部分测定结果如下表所示：
| 样品 | 亚甲基蓝溶液初始浓度(mg/L) | 2h后亚甲基蓝溶液浓度(mg/L) | 3h后亚甲基蓝溶液浓度(mg/L) | 光照2h的降解率（%） | 光照3h的降解率（%） |
| 实施例1 | 8 | 3.681 | 1.587 | 53.988 | 80.162 |
| 实施例2 | 8 | 1.782 | 0.467 | 77.725 | 94.163 |
| 实施例3 | 8 | 1.712 | 0.381 | 78.594 | 95.237 |
| 实施例4 | 8 | 2.951 | 0.466 | 63.111 | 94.174 |
| 实施例5 | 8 | 3.219 | 0.865 | 59.757 | 89.185 |
由表可知，本发明实施例所制备的光催化剂有较高的光催化活性，可见光下对亚甲基蓝的降解率可达到90%以上，具有很好的市场前景。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理和构思的前提下，对本发明的技术方案进行修改或者等同替换也应视为本发明的保护范围。
Claims (6)
1.一种可见光响应型光催化剂，其特征在于：化学式为Ce-Sr2Bi2O5，以氧化铋和碳酸锶为原料，以氧化铈为掺杂剂；其制备方法包括以下步骤：
(1)按照比例称取一定量的氧化铋和碳酸锶于球磨罐里，加入氧化铈；
(2)向上述球罐里加入适量去离子水和球磨玛瑙球；
(3)将上述球罐置于行星球磨机上进行球磨，在一定转速下球磨一段时间后得到的浆料进行干燥；
(4)干燥后的物料研磨过筛，然后置于马弗炉里进行焙烧，反应一段时间后自然降温，待其冷却后研磨过筛得到样品；
(5)将上样品置于马弗炉里进行焙烧，保温一段时间后自然降温，待其冷却后研磨过筛可得到所述可见光响应型光催化剂。
2.根据权利要求1所述的制备方法，其特征在于：上述步骤(1)中氧化铋和碳酸锶的物质的量的比例为1：2，氧化铈与氧化铋物质的量的比例为0.01～0.4。
3.根据权利要求1所述的制备方法，其特征在于：所述步骤(2)玛瑙球与物料比为1～3:1，加去离子水淹没物料且体积为球罐容积的60%～90%。
4.根据权利要求1所述的制备方法，其特征在于：所述步骤(3)转速为200～400r/min，球磨时间为1～3小时。
5.根据权利要求1所述的制备方法，其特征在于：所述步骤(4)焙烧温度为600℃～900℃，保温时间为4h～8h，筛网目数为200～400目。
6.根据权利要求1所述的制备方法，其特征在于：所述步骤(5)焙烧温度为600℃～900℃，保温时间为4h～20h。
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