CN106732683A - 一种合成等离子体复合光催化剂的方法 - Google Patents
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Abstract
本发明涉及多元金属氧化物的改性,特指一种以氯化钠、硝酸银、硝酸铋和钼酸钠为原料制备Ag/AgCl/AgBi(MoO4)2等离子体光催化剂的方法。取等物质的量的硝酸银、硝酸铋分散到去离子水中,再加入钼酸钠水溶液,搅拌混合后,微波水热反应,将得到的沉淀用乙醇和去离子水交替清洗三遍;将得到的AgBi(MoO4)2超声分散在乙二醇中,加入不同物质量的氯化钠,继续搅拌4小时后进行光照还原反应,反应结束后,将沉淀过滤,洗涤,烘干,得到Ag/AgCl/AgBi(MoO4)2等离子体光催化剂。通过在可见光下降解盐酸四环素(TC)实验证明所制备的复合光催化剂具有良好的光催化活性。
Description
技术领域
本发明涉及多金属金属氧化物,特指一种以氯化钾、硝酸银、硝酸铋和钼酸钠为原料制备Ag/AgCl/AgBi(MoO4)2等离子体光催化剂的方法,尤其是一种制备工艺简单,可控性强,产品具有良好可见光催化活性的多金属氧化物纳米复合光催化剂制备方法。
背景技术
半导体光催化剂来能够利用太阳能来处理水体中有机污染物或光分解水具有清洁、环保、可持续的特点。多金属氧化物光催化剂由于独特的电子结构和能带位置的多样化被开发,因而在光催化领域已经成为关注的焦点;然而,现有的多金属氧化物光催化剂的催化活性依然很低,无法满足实际应用的需求,因此通过简单、高效的材料制备、改性方法来提高这类半导体材料电子和空穴的分离效率来进而提高其光催化活性仍是一个富有挑战性的课题。
异质结其由于特殊的能带结构和载流子输送特性,在光催化反应中能有效抑制光生电子和空穴复合,提高量子效率,进而大幅提高光催化剂的催化活性,采用简单可行的离子交换法、光还原法来制备多金属氧化物与Ag/AgCl形成异质结构还没有被报道,目前,还没有关于构建Ag/AgCl/AgBi(MoO4)2等离子体光催化剂及其等离子体共振效应并将其应用于光催化降解四环素的研究。
本发明所采用的微波水热法能耗低、反应快速、产物形貌均匀,异质结合成过程中的离子交换法和光还原法的操作简单、反应条件可控、适用性广等优点,采用微波水热法、离子交换法来合成Ag/AgCl/AgBi(MoO4)2等离子体异质结构,同时调节离子交换过程中不同的氯离子浓度,通过光催化降解盐酸四环素(TC)这种对生态环境危害非常严重的有机物考察所制备的光催化剂的催化活性。
发明内容
本发明目的是提供一种利用微波水热法、离子交换法、光还原法制备的基于多金属氧化物的高效等离子体异质结光催化剂,实现可见光下光催化降解四环素的纳米复合光催化剂的方法。
本发明通过以下步骤实现:
(1)将钼酸铋银纳米粒子分散在乙二醇中后加入氯化钾,搅拌混合均匀后进行离子交换反应,进而得到AgCl/AgBi(MoO4)2等离子体光催化剂,其中氯化钾与AgBi(MoO4)2的摩尔比为1:15-5:3;将得到的样品离心、水洗去除残留的乙二醇后分散在去离子水中光照还原反应,反应结束后,将沉淀过滤,洗涤,干燥,最后得到Ag/AgCl/AgBi(MoO4)2等离子体光催化剂。
进一步地,搅拌混合均匀的时间为4h。
进一步地,光照还原反应条件为:氙灯照射下反应30分钟。
进一步地,所述钼酸铋银纳米粒子的制备方法如下:取等摩尔硝酸银、硝酸铋超声分散在去离子水中形成混合溶液,逐滴加入到摩尔数为硝酸银和硝酸铋总和的钼酸钠的水溶液后得到混合溶液,搅拌均匀后进行微波水热反应,160℃下水热反应5分钟,反应结束后,将沉淀过滤,洗涤,烘干,得到钼酸铋银纳米粒子。
(2)本发明所制备的Ag/AgCl/AgBi(MoO4)2等离子体光催化剂,分散良好,性质稳定。
(3)利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、X光电子能谱仪等仪器对产物进行结构分析,以盐酸四环素溶液为目标污染物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。
附图说明
图1为所制备的Ag/AgCl/AgBi(MoO4)2等离子体光催化剂,AgBi(MoO4)2的XRD衍射谱图。
图2为所制备纯AgBi(MoO4)2纳米粒子(a)和Ag/AgCl/AgBi(MoO4)2等离子体异质结光催化剂的扫描电镜照片(b)和Ag/AgCl/AgBi(MoO4)2等离子体光催化剂X光电子能谱图(c)。
图3为所制备含有0.4mmol氯离子的Ag/AgCl/AgBi(MoO4)2等离子体光催化剂与Ag/AgCl、AgBi(MoO4)2光电流图谱(a)和阻抗分析图谱(b)。
图4为所制备不同比例Ag/AgCl/AgBi(MoO4)2等离子体光催化剂的可见光催化降解四环素溶液的时间-降解率关系。
图5为所制备Ag/AgCl/AgBi(MoO4)2等离子体光催化剂最佳样品的降解循环实验。
具体实施方式
实施例1 Ag/AgCl/AgBi(MoO4)2等离子体光催化剂的制备
将1mmol硝酸银,1mmol硝酸铋超声搅拌后均匀分散在5mL去离子水中,搅拌过程中滴入含2mmol钼酸钠的水溶液;在微波消解仪中采用200W功率,160℃下微波水热反应5分钟;将得到的产物用无水乙醇和去离子水交替洗涤各三遍,得到纳米钼酸铋银;将200mg得到的AgBi(MoO4)2超声分散在乙二醇中,加入不同物质的量的氯化钾,充分搅拌4小时,得到AgCl/AgBi(MoO4)2;将得到的样品离心、水洗去除残留的乙二醇;将得到的样品分散在去离子水中采用氙灯照射30分钟,反应结束后,将沉淀过滤,洗涤,干燥,最后得到Ag/AgCl/AgBi(MoO4)2等离子体光催化剂;控制氯化钾与AgBi(MoO4)2的摩尔比分别为1:15,1:3,2:3,4:3和5:3,得到具有不同浓度比例的Ag/AgCl/AgBi(MoO4)2等离子体光催化剂。
实施例2所制备等离子体光催化剂的表征分析
如图1所示,从图中可以看出,复合后的样品同时具有Ag,AgCl,AgBi(MoO4)2的特征峰,说明我们成功制备出了Ag/AgCl/AgBi(MoO4)2等离子体光催化剂。
如图2所示,(A)图中可以看到纯AgBi(MoO4)2为纳米颗粒,由尺寸为10~20nm的纳米粒子组装而成,尺寸为100nm,(B)图中可以看到AgBi(MoO4)2纳米颗粒的表面由于Ag/AgCl的影响而变得粗糙,形状不规则,纳米颗粒尺寸为120nm,(C)图中图谱显示出Ag,Mo,Bi,Cl,氧元素的存在。
如图3所示,(a)图可以清楚看到Ag/AgCl/AgBi(MoO4)2光照后光电流强度要明显高于Ag/AgCl和AgBi(MoO4)2样品,表明这种催化剂内部电荷的有效分离和对光的良好响应能力,(b)图中的阻抗分析结果表明Ag/AgCl/AgBi(MoO4)2等离子体光催化剂具有最小的阻抗值,这个结果与光电流测试结果一致。
实施例3 Ag/AgCl/AgBi(MoO4)2等离子体光催化剂的可见光催化活性实验
(1)配制浓度为10mg/L的盐酸四环素溶液,将配好的溶液置于暗处。
(2)称取Ag/AgCl/AgBi(MoO4)2等离子体光催化剂100mg(当AgBi(MoO4)2质量为200mg,KCl摩尔数分别为0.02,0.1,0.2,0.4和0.5mmol得到的样品分别记为AC-0.02,AC-0.1,AC-0.2,AC-0.4,AC-0.5,对应摩尔比分别为1:15,1:3,2:3,4:3和5:3),分别置于光催化反应器中,加入100mL步骤(1)所配好的目标降解液,磁力搅拌30min待复合光催化剂分散均匀后,打开水源,光源,进行光催化降解实验。
(3)每10min吸取反应器中的光催化降解液,离心后用于紫外-可见吸光度的测量。
(4)由图4可见所制备的等离子体光催化剂具有优异的可见光催化活性,尤其是氯化钾用量为0.4mmol(摩尔比4:3)时得到的样品降解亚盐酸四环素活性最好,比纯的Ag/AgCl和AgBi(MoO4)2的降解活性都要高。
(5)由图5可见所制备的等离子体光催化剂氯化钾量为0.4mmol(摩尔比4:3)时得到的光催化剂在循环使用五次后依然能够保持良好的降解活性,表明这种复合光催化剂具有良好的稳定性和可重复利用特点。
Claims (7)
1.一种合成等离子体复合光催化剂的方法,其特征在于:将钼酸铋银纳米粒子分散在乙二醇中后加入氯化钾,搅拌混合均匀后进行离子交换反应,进而得到AgCl/AgBi(MoO4)2等离子体光催化剂;将得到的样品离心、水洗去除残留的乙二醇后分散在去离子水中光照还原反应,反应结束后,将沉淀过滤,洗涤,干燥,最后得到Ag/AgCl/AgBi(MoO4)2等离子体复合光催化剂。
2.如权利要求1所述的一种合成等离子体复合光催化剂的方法,其特征在于:氯化钾与AgBi(MoO4)2的摩尔比分别为1:15-5:3。
3.如权利要求2所述的一种合成等离子体复合光催化剂的方法,其特征在于:氯化钾与AgBi(MoO4)2的摩尔比为4:3。
4.如权利要求1所述的一种合成等离子体复合光催化剂的方法,其特征在于:搅拌混合均匀的时间为4h。
5.如权利要求1所述的一种合成等离子体复合光催化剂的方法,其特征在于:光照还原反应条件为:氙灯照射下反应30分钟。
6.如权利要求1所述的一种合成等离子体复合光催化剂的方法,其特征在于,所述钼酸铋银纳米粒子的制备方法如下:取等摩尔硝酸银、硝酸铋超声分散在去离子水中形成混合溶液,逐滴加入到摩尔数为硝酸银和硝酸铋总和的钼酸钠的水溶液后得到混合溶液,搅拌均匀后进行微波水热反应,200W功率,160℃下水热反应5分钟,反应结束后,将沉淀过滤,洗涤,烘干,得到钼酸铋银纳米粒子。
7.如权利要求1所述的一种合成等离子体复合光催化剂的方法,其特征在于,所述的Ag/AgCl/AgBi(MoO4)2等离子体复合光催化剂,AgBi(MoO4)2表面均匀生长AgCl和Ag纳米颗粒。
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