CN113181912B - 一种Cu2O-TiO2复合光催化剂及其制备方法和应用 - Google Patents
一种Cu2O-TiO2复合光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种Cu2O‑TiO2复合光催化剂及其制备方法和应用，该复合光催化剂由Cu2O纳米球和TiO2纳米片按质量比1:2.8组成，Cu2O为空心结构的纳米球，其均匀地负载在TiO2纳米片上。空心结构Cu2O具有更多的活性位点、光吸收能力强、利于反应分子扩散等优点；TiO2纳米片具有氧化能力高的表面和比表面大等优势。二者优势协同增强，Cu2O‑TiO2的光催化性能得到大幅度提高。与TiO2比较，其活性提高了1.64倍。本发明的Cu2O‑TiO2复合光催化剂紫外光下能够很好降解甲基橙(MO)废水溶液，其制作方法简易，成本低廉，重现性好，结构独特，因此具有良好的应用前景。
Description
技术领域
本发明属于光催化材料技术领域，具体涉及一种Cu2O-TiO2复合光催化剂及其制备方法和应用。
背景技术
随着经济的发展和社会的进步，环境污染问题日益加剧。当前，全球十大环境问题之一的水体污染问题日益引起人们的重视。水体污染物主要是有机污染物、病原体污染物和有毒污染物等，人们采用了多种方法处理废水，主要包括物理方法、化学方法和生物方法等。与其他方法相比，光催化利用丰富的太阳能，能够彻底分解毒性有机污染物，不产生二次污染。该技术不消耗化石资源，具有操作简单、成本低等优势。
光催化反应的技术核心，是制造高效、廉价的光催化剂。在数千种光催化剂中，TiO2是最高效的紫外响应型光催化剂之一，因其成本低、无毒、稳定性高而受到人们的特别关注。但其光吸收范围较窄，太阳光中的紫外光比例不到5％，其余部分为可见光和红外光，因此，无法充分利用太阳能。此外，TiO2的光生电子与空穴的复合率高，其光催化效率仍然无法满足实际需要。到目前为止，科学家研究开发了离子掺杂、半导体复合、金属修饰等多种方法，改善二氧化钛的性能。在已有的报道中，许成群等人报道了g-C3N4/TiO2光催化剂材料(申请公布号：202011157436.3)。但空心结构纳米球负载于纳米片的Cu2O-TiO2复合材料，迄今尚未报道。
发明内容
针对现有技术的不足，本发明提供一种Cu2O-TiO2复合光催化剂及其制备方法和应用，制作方法简易，成本低廉，重现性好，结构独特，紫外光下能够很好降解甲基橙(MO)废水溶液。
本发明是通过以下技术方案实现的：
一种Cu2O-TiO2复合光催化剂，所述复合光催化剂由Cu2O纳米球和TiO2纳米片按质量比1:2.8组成，所述Cu2O纳米球为空心结构的纳米球，所述空心结构的纳米球均匀地负载在所述TiO2纳米片上。
优选地，所述TiO2纳米片的边长为1.7μm，厚度为160～250nm；Cu2O纳米球的直径为112～275nm。
一种Cu2O-TiO2复合光催化剂的制备方法，包括以下步骤：
步骤1)在容器中按质量比6.3:60.03:0.5加入水、冰醋酸和氢氟酸，搅拌均匀，然后加入1.7g钛酸四丁酯，搅拌30min；
步骤2)将步骤1)得到的混合溶液转移到聚四氟乙烯内衬中，180℃恒温水热反应24h，之后自然冷却至室温，离心洗涤、干燥，产物为纯相TiO2；
步骤3)取0.08g步骤2)所得的纯相TiO2加入到100mL水中，在60℃的水浴条件下缓慢加入4.786g十六烷基三甲基溴化铵，然后加入0.05g五水硫酸铜和0.18g抗坏血酸，搅拌20min，再滴加10mL 0.2mol/L NaOH，搅拌10min后，离心洗涤、干燥，产物即为所述Cu2O-TiO2复合光催化剂。
优选地，步骤1)所述氢氟酸的质量分数为40wt％。
一种Cu2O-TiO2复合光催化剂在降解废水中有机染料上的应用。
优选地，所述有机染料为甲基橙。
本发明的有益效果如下：
本发明采用温和原位还原法制备了Cu2O-TiO2复合光催化剂，产品具有独特的微观结构——空心结构纳米球负载于纳米片，能够充分发挥各组分的优势。空心结构Cu2O具有更多的活性位点、光吸收能力强、利于反应分子扩散等优点；TiO2纳米片具有氧化能力高的表面和比表面大等优势。二者优势协同增强，Cu2O-TiO2的光催化性能得到大幅度提高。与TiO2比较，其活性提高了1.64倍。本发明的Cu2O-TiO2复合光催化剂紫外光下能够很好降解甲基橙(MO)废水溶液，其制作方法简易，成本低廉，重现性好，结构独特，因此具有良好的应用前景。
附图说明
图1为实施例1制得的TiO2和Cu2O-TiO2的X射线衍射(XRD)图；
图2为实施例1制得的TiO2的扫描电子显微镜(SEM)图；
图3为实施例1制得的Cu2O-TiO2的扫描电子显微镜(SEM)图；
图4为实施例1制得的Cu2O-TiO2的高分辨电子显微镜(HRTEM)图；
图5为测试例1中TiO2和Cu2O-TiO2分别对甲基橙(MO)染料废水溶液降解的活性对比图。
具体实施方式
下面结合附图与实施例对本发明做进一步详细说明。
实施例1
一种Cu2O-TiO2复合光催化剂，所述复合光催化剂由Cu2O纳米球和TiO2纳米片按质量比1:2.8组成，所述Cu2O纳米球为空心结构的纳米球，所述空心结构的纳米球均匀地负载在所述TiO2纳米片上。
一种Cu2O-TiO2复合光催化剂的制备方法，具体步骤如下：
(1)室温下，在烧杯中，加入3.15g水、30.03g冰醋酸和0.5g 40wt％的氢氟酸，搅拌均匀，然后加入1.7g的钛酸四丁酯(TBOT)，搅拌30min。
(2)将得到的混合溶液转移到聚四氟乙烯内衬中，180℃恒温水热反应24h，反应24h后，自然冷却至室温，离心洗涤、干燥，产物为TiO2。
(3)将0.08g产物放到装有100mL水的烧杯中，在60℃的水浴条件下缓慢加入4.786g的十六烷基三甲基溴化铵(CTAB)，然后加入0.05g五水硫酸铜和0.18g抗坏血酸，搅拌20min后，缓慢滴加10mL 0.2mol/L的NaOH，搅拌10min后，离心洗涤、干燥，产物即为所述Cu2O-TiO2复合光催化剂。
图1为步骤(2)制得的纳米片TiO2和最终产物Cu2O-TiO2复合光催化剂的X射线衍射(XRD)图。由图1可见，本实施例制得的产品TiO2材料和Cu2O-TiO2分别与TiO2标准卡(PDF#21-1272)一致，Cu2O与Cu2O标准卡(PDF#34-1354)一致，证实本实施例制得的产品分别是纯相的TiO2材料和含微量Cu2O的Cu2O-TiO2材料以及纯相Cu2O材料。
图2为步骤(2)制得的TiO2的扫描电子显微镜(SEM)图。由图2可见，本实施例所制备的TiO2形貌为纳米片，片厚度为160～250nm，纳米片大小为1.7μm×1.7μm左右。
图3为最终产物Cu2O-TiO2复合光催化剂的扫描电子显微镜(SEM)图。由图3可见，本实施例所制备的Cu2O-TiO2复合光催化剂形貌为球状，Cu2O均匀负载在纳米片TiO2上，球体直径为112～275nm。
图4为最终产物Cu2O-TiO2复合光催化剂的高分辨电子显微镜(HRTEM)图。由图4可见，本实施例所制备的Cu2O-TiO2复合光催化剂形貌为空心球状，Cu2O均匀负载在纳米片TiO2上。
测试例1
将实施例1制得的Cu2O-TiO2复合光催化剂、纯相的TiO2，用于降解含有甲基橙(MO)的废水溶液。测试过程如下：
称取Cu2O-TiO2复合光催化剂、纯相的TiO2的样品各0.02g，分别加入200mL的MO水溶液，其中MO浓度均为12.5mg/L，先避光搅拌30min，使染料在催化剂表面达到吸附/脱附平衡。然后开启氙灯光源在紫外光照射下进行光催化反应，上清液用分光光度计检测。
根据Lambert-Beer定律，有机物特征吸收峰强度的变化，可以定量计算其浓度变化。当吸光物质相同、厚度相同时，可以用吸光度的变化直接表示溶液浓度的变化。因为MO在463nm处有一个特征吸收峰，所以可以利用吸光度的变化来衡量溶液中MO的浓度变化。图5中，横坐标为紫外光照射时间，纵坐标为经过紫外光照射一段时间后测量的MO浓度值(C)与MO的初始浓度(C0)的比值。从图5可以看出，实施例1合成的Cu2O-TiO2复合光催化剂的活性，相较于纯相TiO2提高了1.64倍。
Claims (4)
1.一种Cu2O-TiO2复合光催化剂的制备方法，其特征在于，所述复合光催化剂由Cu2O纳米球和TiO2纳米片按质量比1:2.8组成，所述Cu2O纳米球为空心结构的纳米球，所述空心结构的纳米球均匀地负载在所述TiO2纳米片上；所述TiO2纳米片的边长为1.7μm，厚度为160～250nm；Cu2O纳米球的直径为112～275nm；制备方法包括以下步骤：
步骤1)在容器中按质量比6.3:60.03:0.5加入水、冰醋酸和氢氟酸，搅拌均匀，然后加入1.7g钛酸四丁酯，搅拌30min；
步骤2)将步骤1)得到的混合溶液转移到聚四氟乙烯内衬中，180℃恒温水热反应24h，之后自然冷却至室温，离心洗涤、干燥，产物为纯相TiO2；
步骤3)取0.08g步骤2)所得的纯相TiO2加入到100mL水中，在60℃的水浴条件下缓慢加入4.786g十六烷基三甲基溴化铵，然后加入0.05g五水硫酸铜和0.18g抗坏血酸，搅拌20min，再滴加10mL 0.2mol/L NaOH，搅拌10min后，离心洗涤、干燥，产物即为所述Cu2O-TiO2复合光催化剂。
2.根据权利要求1所述的一种Cu2O-TiO2复合光催化剂的制备方法，其特征在于，步骤1)所述氢氟酸的质量分数为40wt％。
3.权利要求1所述制备方法制得的Cu2O-TiO2复合光催化剂在降解废水中有机染料上的应用。
4.根据权利要求3所述的应用，其特征在于，所述有机染料为甲基橙。
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