CN110694620A - 一种Ag-HSTiO2复合结构催化剂的制备方法 - Google Patents
一种Ag-HSTiO2复合结构催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种Ag‑HSTiO2复合结构催化剂的制备方法,属于纳米材料制备与应用技术领域。将Ag纳米颗粒与具紫外光催化活性的高比表面积TiO2(HSTiO2)复合作为催化降解工业有机染料的催化剂,由于复合物发挥了Ag纳米颗粒尺寸小,以及HSTiO2的稳定性能、反应接触面积大和紫外光响应等优点。使Ag纳米颗粒与HSTiO2之间发生协同作用,提高量子产率,拓宽了光响应范围。采用紫外可见光谱仪对催化性能进行检测,并可确定催化剂在反应结束后是否失活以及催化剂循环使用情况。本发明方法简单、环保、低成本;催化效果明显,反应迅速,具有可重复性高等优点;此催化剂对可见光催化降解染料废水具有潜在应用价值。
Description
技术领域
本发明属于纳米材料的制备及应用领域,具体的说涉及一种Ag-HSTiO2复合结构催化剂的制备方法及该催化剂在可见光下催化甲基橙降解的应用。
背景技术
经济发展和工业化带动了人民生活水平的迅速提高。同时暴露出严重的环境污染问题,导致环境恶化,威胁人类健康,阻碍可持续发展。科学技术的发展带动了半导体光催化技术的进步,半导体光催化技术已成为研究的热点,并能有效地解决这些问题。
TiO2作为光催化半导体材料具有以下优点。首先,TiO2安全无毒。其次,TiO2广泛存在于地壳中。第三,TiO2价格便宜,生产成本低。值得注意的是,TiO2的缺点也很明显。例如,TiO2可以吸收大部分紫外线,但它只能吸收一小部分可见光,其光生电子很容易重组。在TiO2表面沉积Au、Pt和Ag等贵金属,可以降低电子空穴的复合速率和转移光生电子。然而贵金属价格普遍较高,为了节省成本通常选择Ag。值得注意的是,Ag纳米颗粒在光催化反应中很容易聚集,经过多次反应后会失去活性。因此,研究人员将Ag纳米颗粒负载到半导体TiO2表面形成复合材料。该策略可以有效地将TiO2的光谱响应范围从紫外区域扩展到可见区域。此外,该策略还可以防止Ag纳米颗粒的团聚,从而协同提高光催化活性。然而,这些方法存在以下问题。一是制备过程能耗大。二是制备工艺复杂,得到的产品较少。三是循环稳定性差,产品难以重复使用。为了解决这些问题,提高TiO2的光催化活性,研究人员提出了增加TiO2的比表面积,以暴露更多的活性中心。
发明内容
本发明的目的是克服现有技术的不足,提供一种新的制备Ag-HSTiO2复合结构催化剂的方法,该方法简单易行,所制备的催化剂具有更强的可见光催化作用。
本发明的目的是这样实现的:该催化剂的制备包括以下步骤:
(1)、高比表面积二氧化钛(HSTiO2)的制备,将1.6g的F127[聚(乙二醇)-block-聚(丙二醇)-block-聚(乙二醇)]加入30mL浓度大于99.9%的乙醇溶液中,60℃下搅拌30分钟,转速为300rpm,使其充分溶解;再向溶液中依次加入0.7mL浓度大于99.5%的盐酸、2.3mL浓度大于99.5%的乙酸、3.5mL浓度大于99.5%的钛酸四丁酯继续搅拌30分钟,转速仍然为300rpm;随后将装有混合溶液的烧杯放入电热鼓风干燥箱中,60℃下烘干24小时后得到二氧化钛凝胶后将样品放入马弗炉中,以5℃/min的速率升温到450℃,保温4小时,冷却后研磨得到高比表面积纳米结构二氧化钛。
(2)、银-高比表面积二氧化钛复合物(Ag-HSTiO2)的制备,将0.8g制备好的高比表面积二氧化钛样品与0.12g硝酸银加入100mL烧杯中,再向烧杯中加入40mL浓度大于99.5%的甲醇溶液,黑暗下搅拌30分钟,转速为300rpm,使其混合均匀;随后使用500W氙灯照射烧杯30分钟,氙灯距离烧杯20厘米,使其充分反应;反应后将溶液等体积分成两份分别转移到两个50mL的离心试管中,再将离心试管放入高速离心机中离心,离心的转速为5000rmp,离心时间为5分钟;离心完成后弃上清液,再向两个离心试管中分别加入20mL的去离子水后,将两个离心试管放入超声波清洗器中超声3分钟,超声完毕将两个试管放入高速离心机中离心5分钟,离心转速为5000rmp,弃上清液,重复上述用去离子水洗涤过程两次,洗涤完成后将样品放入电热鼓风干燥箱中60℃干燥12h,得到银-高比表面积二氧化钛复合物(Ag-HSTiO2)。
本发明具有以下优点和积极效果:
1、本发明方法合成的催化剂样品合成工艺简便、样品纯度高,首次采用光沉积法将银纳米颗粒沉积在高比表面积二氧化钛表面,从而获得Ag-HSTiO2复合光催化剂。从图1的XRD图像可以看出,所制备出的样品所有衍射峰位置都对应Ag以及TiO2的峰,无杂质峰,说明制备出的Ag-HSTiO2光催化剂纯度高。图2是Ag-HSTiO2的N2吸附脱附曲线,从曲线可以得知所制备的样品比表面积高。图3是Ag-HSTiO2的SEM图像,从图像可以看出所制备出的样品是Ag与TiO2的复合结构。图4、5是Ag-HSTiO2的光催化降解甲基橙实验以及循环实验的结果,从图4、5中可以看出所制备的复合光催化剂降解甲基橙催化效果良好,经过5次循环测试后仍能保持90%以上的活性,说明样品的循环稳定性好。
2、本发明的方法并未使用大功率仪器,能耗低,而且在整个实验过程中并未产生有毒有害气体,安全环保。
3、本发明产品通过五个循环测试,仍然能将甲基橙降解90%以上,说明样品的循环稳定性好,可以重复利用。
附图说明
图1是本发明Ag-HSTiO2的XRD测试结果图;
图2是本发明Ag-HSTiO2的N2吸附脱附曲线图;
图3是本发明Ag-HSTiO2的扫描电镜照片图像;
图4是本发明Ag-HSTiO2的光催化降解甲基橙实验结果图。
图5是本发明Ag-HSTiO2的光催化降解甲基橙循环试验结果。
具体实施方式
本发明的目的是这样实现的:该催化剂的制备方法包括以下步骤:
(1)、高比表面积二氧化钛(HSTiO2)的制备,将1.6g的F127[聚(乙二醇)-block-聚(丙二醇)-block-聚(乙二醇)]加入30mL浓度大于99.9%的乙醇溶液中,60℃下搅拌30分钟,转速为300rpm,使其充分溶解;再向溶液中依次加入0.7mL浓度大于99.5%的盐酸、2.3mL浓度大于99.5%的乙酸、3.5mL浓度大于99.5%的钛酸四丁酯继续搅拌30分钟,转速仍然为300rpm;随后将装有混合溶液的烧杯放入电热鼓风干燥箱中,60℃C下烘干24小时后得到二氧化钛凝胶后将样品放入马弗炉中,以5℃/min的速率升温到450℃,保温4小时,冷却后研磨得到高比表面积纳米结构二氧化钛。
(2)、银-高比表面积二氧化钛复合物(Ag-HSTiO2)的制备,将0.8g制备好的高比表面积二氧化钛样品与0.12g硝酸银加入100mL烧杯中,再向烧杯中加入40mL浓度大于99.5%的甲醇溶液,黑暗下搅拌30分钟,转速为300rpm,使其混合均匀;随后使用500W氙灯照射烧杯30分钟,氙灯距离烧杯20厘米,使其充分反应;反应后将溶液等体积分成两份分别转移到两个50mL的离心试管中,再将离心试管放入高速离心机中离心,离心的转速为5000rmp,离心时间为5分钟;离心完成后弃上清液,再向两个离心试管中分别加入20mL的去离子水后,将两个离心试管放入超声波清洗器中超声3分钟,超声完毕将两个试管放入高速离心机中离心5分钟,离心转速为5000rmp,弃上清液,重复上述用去离子水洗涤过程两次,洗涤完成后将样品放入电热鼓风干燥箱中60℃干燥12h,得到银-高比表面积二氧化钛复合物(Ag-HSTiO2)。
采用X射线衍射(XRD)、扫描电子显微镜、可见分光光度计及BET表征上述方法制备的Ag-HSTiO2光催化剂,从图1样品的XRD图像可以看出,Ag-HSTiO2复合物所有的衍射峰位置都对应Ag和TiO2的衍射峰,并且无任何杂质峰,说明所制备出的Ag-HSTiO2催化剂纯度很高;从图2Ag-HSTiO2复合物N2吸附脱附曲线计算得出,所制备的Ag-HSTiO2复合物比表面积为86.6m2/g,表明Ag-HSTiO2具有高比表面积。从图3扫描电子显微镜图像可以产出,所制备出的样品是Ag-HSTiO2复合物。从图4、5的光催化甲基橙降解实验结果可以看出,Ag-HSTiO2具有良好的催化活性,并且在重复5个循环之后仍能维持90%以上的催化活性。
1、上述步骤(1)(2)中试剂用量不可按比例放大。
2、上述步骤(1)(2)中试剂均为分析纯,未经过进一步处理。
Claims (2)
1.一种Ag-HSTiO2复合结构催化剂的制备方法,其特征在于:该方法包括以下步骤:
(1)、高比表面积二氧化钛(HSTiO2)的制备,将1.6g的F127[聚(乙二醇)-block-聚(丙二醇)-block-聚(乙二醇)]加入30mL浓度大于99.9%的乙醇溶液中,60℃下搅拌30分钟,转速为300rpm,使其充分溶解;再向溶液中依次加入0.7mL浓度大于99.5%的盐酸、2.3mL浓度大于99.5%的乙酸、3.5mL浓度大于99.5%的钛酸四丁酯继续搅拌30分钟,转速仍然为300rpm;随后将装有混合溶液的烧杯放入电热鼓风干燥箱中,60℃下烘干24小时后得到二氧化钛凝胶后将样品放入马弗炉中,以5℃/min的速率升温到450℃,保温4小时,冷却后研磨得到高比表面积纳米结构二氧化钛;
(2)、银-高比表面积二氧化钛复合物(Ag-HSTiO2)的制备,将0.8g制备好的高比表面积二氧化钛样品与0.12g硝酸银加入100mL烧杯中,再向烧杯中加入40mL浓度大于99.5%的甲醇溶液,黑暗下搅拌30分钟,转速为300rpm,使其混合均匀;随后使用500W氙灯照射烧杯30分钟,氙灯距离烧杯20厘米,使其充分反应;反应后将溶液等体积分成两份分别转移到两个50mL的离心试管中,再将离心试管放入高速离心机中离心,离心的转速为5000rmp,离心时间为5分钟;离心完成后弃上清液,再向两个离心试管中分别加入20mL的去离子水后,将两个离心试管放入超声波清洗器中超声3分钟,超声完毕将两个试管放入高速离心机中离心5分钟,离心转速为5000rmp,弃上清液,重复上述用去离子水洗涤过程两次,洗涤完成后将样品放入电热鼓风干燥箱中60℃干燥12h,得到银-高比表面积二氧化钛复合物(Ag-HSTiO2)。
2.一种如权利要求1所述一种Ag-HSTiO2复合结构催化剂在可见光下催化甲基橙降解的应用。
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