CN107138148A - 一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂及其制备方法 - Google Patents
一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明属于光催化技术领域，涉及一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂及其制备方法；本发明首先量取钛酸四丁酯、乙酰丙酮和硝酸铋于烧杯中，加入冰醋酸搅拌溶解；再将溶液倒入蒸发皿中，放置在烘箱内制得前驱体粉末；经过煅烧，得到Bi2Ti2O7/Bi4Ti3O12复合光催化剂；本方法通过化学溶液分解法制备前驱体粉末，通过煅烧得到混晶材料，产品具有粒径小、形貌规则、可见光吸收能力高，光催化效果好等优点；并且反应条件易控制、工艺和流程简便、能耗低。
Description
技术领域
本发明属于光催化技术领域，涉及一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂及其制备方法，具体涉及一种以硝酸铋和钛酸四丁酯为铋源和钛源，通过化学溶液分解法制备Bi2Ti2O7/Bi4Ti3O12复合光催化剂的方法。
背景技术
近年来，可见光催化技术由于在太阳能转换和环境净化方面的巨大潜力，受到广泛的关注。自从TiO2被发现可以作为潜在的光催化半导体，应用于污染物降解和分解水制氢，科学家们尝试了各种方法来改善其光催化性能。然而，受限于两个主要的缺点：可见光利用率低和光生电子空穴复合率高，TiO2仍然很难实现对可见光的高效利用。因此，研究人员专注于找到其他有着更好的光催化活性的半导体。
Bi4Ti3O12是一种典型的aurivillius氧化物半导体,与二氧化钛相比(E g=3.2 eV)光学带隙较低(E g=2.8 eV)。由于结构中存在TiO4四面体和立体活性的Bi3＋离子，它作为一种新型高效光催化剂在近年来被广泛研究。但是有关Bi4Ti3O12基的混晶材料的研究目前还很少。Du等(Phys. Chem. Chem. Phys., 2016, 18(38), 26530) 将不同摩尔比的锐钛矿TiO2和Bi2O3混合均匀，在750℃下煅烧2h，制得Bi12TiO20/Bi4Ti3O12复合光催化剂。Liu等(J.Mater. Sci-Mater. El. 2016, 1, 16)将P25，Bi2O3，NaCl，KCl以一定的比例研磨均匀，在900℃下煅烧2h，得到Bi2Ti2O7/Bi4Ti3O12纳米片异质结。Shi等(J. Mater. Chem. A, 2015,3(12), 6586)将硝酸铋和钛酸四丁酯溶解在DMF中，以PVP为表面活性剂，通过静电纺丝法制得了Bi2Ti2O7/Bi4Ti3O12纳米纤维异质结。然而这些方法对设备的要求高，并且得到的钛酸铋基混晶材料颗粒巨大，严重影响了其光催化活性。所以开发操作简单，成本低廉，粒径微小，适用于大规模生产的方法，已经成为Bi2Ti2O7/Bi4Ti3O12复合光催化剂生产者们所追求的主要目标。
发明内容
本发明的目的在于克服现有技术中存在的技术缺陷，提供一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂，以及一种化学溶液分解法制备Bi2Ti2O7/Bi4Ti3O12复合光催化剂的方法。
本发明首先提供一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂，该催化剂为一种纳米颗粒，该催化剂粒径较小，粒径仅为20-80 nm、形貌规则、可见光吸收能力高、光催化效果好。
本发明还提一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂的制备方法，通过以下步骤实现：
（1）量取钛酸四丁酯，乙酰丙酮和一定量的硝酸铋于烧杯中，加入冰醋酸搅拌溶解；
（2）将溶液倒入蒸发皿中，放置在烘箱内制得前驱体粉末；
（3）将步骤（2）得到的前驱体粉末经过煅烧，得到Bi2Ti2O7/Bi4Ti3O12复合光催化剂。
步骤（1）中，钛酸四丁酯、乙酰丙酮和硝酸铋的用量为0.5 mL ：0.5 mL ：0.6~1.1g。
步骤（2）中，烘箱的温度范围为140~180℃，反应时间5~10 h。
步骤（3）中，所述煅烧温度为550~650℃，煅烧时间为0.5~4h。
本发明所制得的Bi2Ti2O7/Bi4Ti3O12复合光催化剂，晶化完全，粒径较小，分散性好。
利用X射线衍射仪（XRD）、透射电子显微镜（TEM）、紫外-可见分光度计（DRS）对产物进行形貌结构分析，以盐酸四环素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。
本发明具有以下优点：
（1）本方法采用化学溶液分解法制备前驱体粉末，通过煅烧得到混晶材料。与直接煅烧法采用的Bi2O3和TiO2为原料不同，本方法选择硝酸铋和钛酸四丁酯为原料，先制备前驱体，后生成钛酸铋。与直接煅烧法相比，得到的钛酸铋粒径更小。这是由于在前驱体中，存在大量的有机成分，这些成分可以在煅烧过程中阻碍晶体的团聚，从而得到更小粒径的钛酸铋。并且本方法反应条件易控制、工艺和流程简便、反应的低能耗低，不需要静电纺丝法中的大功率的昂贵的纺线仪器和近一天的纺线时间，更有利于工业化应用。
（2）用此方法制备的Bi2Ti2O7/Bi4Ti3O12复合光催化剂，具有粒径较小、形貌规则、可见光吸收能力高，光催化效果好等优点。其中较小的粒径可以为光催化反应提供更多的反应位点；也可以提高Bi2Ti2O7与Bi4Ti3O12这两种半导体之间的接触面积，从而提供更多的异质结结构，增强电子空穴分离效率；同时这种结构还提高了所制备催化剂的可见光吸收能力。综合这三大优势，本材料在光催化降解实验中，表现出明显增强的活性。
附图说明
图1为所制备Bi2Ti2O7/Bi4Ti3O12复合光催化剂的XRD衍射谱图，图中衍射峰均为Bi2Ti2O7或者Bi4Ti3O12特征衍射峰。
图2为所制备Bi2Ti2O7/Bi4Ti3O12复合光催化剂的透射电镜照片。
图3为所制备Bi2Ti2O7/Bi4Ti3O12的固体紫外曲线。
图4为Bi2Ti2O7、/Bi4Ti3O12和Bi2Ti2O7/Bi4Ti3O12复合光催化剂降解盐酸四环素溶液的时间-降解率关系图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1：
在50 mL的烧杯中加入20 mL冰醋酸溶液，再加入0.8g硝酸铋，磁力搅拌至溶解，用微量进样器分别加入0.5mL乙酰丙酮和0.5ml钛酸四丁酯，待反应物混合均匀后，将溶液倒入蒸发皿中，180℃蒸发10 h。将所得的粉末置于坩埚中，在650℃煅烧2h。
图1为制得的样品的XRD衍射谱图，图中衍射峰均为Bi2Ti2O7或者Bi4Ti3O12特征衍射峰，对比标准JCPDS 卡片(32-0118,21-1272), 可以确定为结晶性良好的Bi2Ti2O7/Bi4Ti3O12粉体，图2为所制备的复合光催化剂的透射电镜照片，图中较大颗粒为Bi4Ti3O12颗粒，较小颗粒为Bi2Ti2O7，从图中可以看到Bi2Ti2O7和Bi4Ti3O12之间结合紧密，粒径较小，大约为20-80 nm，大小均匀。图3为所制备的复合光催化剂的固体紫外曲线，相比单一的Bi2Ti2O7和Bi4Ti3O12，Bi2Ti2O7/Bi4Ti3O12复合物的可见光吸收范围有着明显的红移。
现有技术中涉及到的Bi2Ti2O7/Bi4Ti3O12纳米纤维，是一种直径100nm，长度为十几μm的线状材料；而本发明中得到的是Bi2Ti2O7/Bi4Ti3O12纳米颗粒，粒径仅为20-80 nm。更小的粒径可以为光催化反应提供更多的反应位点；也可以提高Bi2Ti2O7与Bi4Ti3O12这两种半导体之间的接触面积，从而提供更多的异质结结构，增强电子空穴分离效率；同时这种结构还提高了所制备催化剂的可见光吸收能力。图3中可以看到所得材料吸收范围出现明显的红移，既表明其可见光吸收能力得到的增强。
实施例2：
在50 mL的烧杯中加入20 mL冰醋酸溶液，再加入0.6g硝酸铋，磁力搅拌至溶解，用微量进样器分别加入0.5mL乙酰丙酮和0.5ml钛酸四丁酯，待反应物混合均匀后，将溶液倒入蒸发皿中，140℃蒸发5 h。将所得的粉末置于坩埚中，在550℃煅烧0.5h。
实施例3：
在50 mL的烧杯中加入20 mL冰醋酸溶液，再加入0.8g硝酸铋，磁力搅拌至溶解，用微量进样器分别加入0.5mL乙酰丙酮和0.5ml钛酸四丁酯，待反应物混合均匀后，将溶液倒入蒸发皿中，140℃蒸发5h。将所得的粉末置于坩埚中，在600℃煅烧1h。
实施例4：
在50 mL的烧杯中加入20 mL冰醋酸溶液，再加入1.1g硝酸铋，磁力搅拌至溶解，用微量进样器分别加入0.5mL乙酰丙酮和0.5ml钛酸四丁酯，待反应物混合均匀后，将溶液倒入蒸发皿中，150℃蒸发7 h。将所得的粉末置于坩埚中，在550℃煅烧4h。
实施例5：
（1）配制浓度为 10 mg/L的盐酸四环素溶液，将配好的溶液置于暗处。
（2）称取制备的催化剂 0.1 g，置于光反应器中，加入 100 mL步骤（1）所配好的盐酸四环素溶液，磁力搅拌 30 min，鼓泡，暗反应 1 h, 待催化剂分散均匀后，打开水源，光源，进行光催化降解实验。
（3）每 10 min取样一次，取样量为 5 ml，用多管架自动平衡离心机离心 3 min,使催化剂完全沉淀，离心后用于紫外-可见吸光度的测量。
（4）由图4可见所制备的复合光催化剂具有优异的光催化活性，反应 40 min，对盐酸四环素的降解率接近 95 %，其性能优于单一的Bi2Ti2O7和Bi4Ti3O12。
目前现有技术中的材料光催化降解染料的活性并不十分突出，有的在在光照5h后，仅仅降解50%甲基橙染料；而本发明中得到的材料可以在40min后，降解95%污染物。
Claims (9)
1.一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂，其特征在于，所述催化剂为一种纳米颗粒，粒径较小，仅为20-80 nm，形貌规则。
2.一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂的制备方法，通过以下步骤实现：
量取钛酸四丁酯，乙酰丙酮和一定量的硝酸铋于烧杯中，加入冰醋酸搅拌溶解；
将溶液倒入蒸发皿中，放置在烘箱内制得前驱体粉末；
将步骤（2）得到的前驱体粉末经过煅烧，得到Bi2Ti2O7/Bi4Ti3O12复合光催化剂。
3.根据权利要求2所述的制备方法，其特征在于，步骤（1）中所述的钛酸四丁酯、乙酰丙酮和硝酸铋的用量为0.5 mL ：0.5 mL ：0.6~1.1g。
4.根据权利要求2所述的制备方法，其特征在于，步骤（2）中所述烘箱的温度范围为140~180℃。
5.根据权利要求2所述的制备方法，其特征在于，步骤（2）中所述烘箱内反应时间5~10h。
6.根据权利要求2所述的制备方法，其特征在于，步骤（3）中所述煅烧温度为550~650℃。
7.根据权利要求2所述的制备方法，其特征在于，步骤（3）中所述煅烧时间为0.5~4h。
8.一种Bi2Ti2O7/Bi4Ti3O12复合光催化剂在环境净化中的应用。
9.根据权利要求8所述的应用，其特征在于，所述应用为对盐酸四环素的降解。
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| CN109999785A (zh) * | 2019-05-13 | 2019-07-12 | 兰州理工大学 | Bi4Ti3O12/Bi2Ti2O7复合光催化剂的制备方法 |
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