CN111905762A - 一种Pt/Bi2WO6/CuS三元复合光催化剂及其制备方法 - Google Patents
一种Pt/Bi2WO6/CuS三元复合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Pt/Bi2WO6/CuS三元复合光催化剂及其制备方法。该三元复合光催化剂中的Pt弥散分布在Bi2WO6/CuS纳米微球(BWC4‑1)的表面,并使两相界面之间形成异质结结构。本发明的制备原料均为常用无机化学试剂、价廉易得,方法工艺简单、对设备的要求较低、可快速合成异质结催化剂,过程简易反应条件可控性强。所制备的Pt/Bi2WO6/CuS光催化剂具有较高的结晶性,且无其他杂质产生,Pt光量子点的加入拓宽了可见光的吸收范围,具有比单一BWC4‑1更优异的可见光催化活性。
Description
技术领域
本发明属于水、气处理技术和环境功能材料领域,具体涉及一种Pt/Bi2WO6/CuS三元复合光催化剂及其制备方法。
背景技术
医药、印染、造纸等工业有机废水排放量大、且含有大量对人体健康能够产生长远不良影响的难降解污染物,是造成水生态环境破坏、严重影响水资源利用的重大污染源。光催化技术可利用半导体光催化材料将“绿色”的太阳能转化为化学能或电能,在温和的反应条件下有效去除水体中的有机污染物,是解决能源和环境问题最有潜力的技术之一。
近年来,为了提高半导体催化材料的光催化活性和稳定性,国内外研究者开发了大量新型光催化材料,如构筑型新型化合物、多元金属氧化物、层状化合物、金属氢氧化物等。Bi2WO6作为作为少有的几个在可见光照射下可以光解水,又可以用来降解有机污染物的光催化剂是近年来光催化领域研究的热点。然而传统Bi2WO6在酸性条件下会分解成钨酸,稳定性不高,难以满足实际应用的要求。因此,必须采取合适的措施来提高CuS/Bi2WO6的抗酸性,提高其稳定程度,从而使得反应能够顺利进行。CuS的带隙为1.76eV~2.48eV,也具有一定的光催化性能,但其在光催化反应中对光的响应度以及光生载流子的迁移效率并不是很高,也是近年来研究的较多的光催化剂之一。将Bi2WO6与CuS复合形成异质结得到具有一定光催化表现的BWC4-1复合光催化剂,但是其对可见光的利用效率不高,且在全光条件下光催化效率不如其他一些新型光催化剂,仍然无法满足实际应用的需要,为了进一步提高其光催化效果,可以在其表面负载一些光量子点,来拓宽催化剂的光响应范围以及光响应强度。
发明内容
针对现有技术中的上述不足,本发明提供一种Pt/Bi2WO6/CuS三元复合光催化剂及其制备方法,可在不需要表面活性剂和复杂的工艺的条件下无污染制备出Pt/Bi2WO6/CuS三元复合光催化剂,并能有效提升催化剂的催化效率和响应。
为实现上述目的,本发明解决其技术问题所采用的技术方案是:
一种Pt/Bi2WO6/CuS三元复合光催化剂,三元复合光催化剂中的Pt弥散分布在Bi2WO6/CuS纳米微球(BWC4-1)的表面,并使两相界面之间形成异质结结构;Pt为Bi2WO6/CuS纳米微球的摩尔质量的0.5~2.5%。
进一步地,Pt与Bi2WO6和/或CuS之间形成异质结。
进一步地,Pt为Bi2WO6/CuS纳米微球的摩尔质量的2.0%。
进一步地,Bi2WO6/CuS纳米微球中Bi2WO6和CuS的摩尔质量比为4:1。
一种上述三元复合光催化剂的制备方法,包括以下步骤:
(1)用有机溶剂溶解Bi2WO6/CuS纳米微球,然后在搅拌的过程中加入氯铂酸,再将其置于功率为250~400W的紫外光下搅拌反应90~120min;所述氯铂酸析出的铂单质为Bi2WO6/CuS纳米微球摩尔质量的0.5~2.5%;
(2)反应完成后过滤并收集洗涤固相产物,再于80~120℃风干,得该三元复合光催化剂。
进一步地,氯铂酸析出的铂单质为Bi2WO6/CuS纳米微球摩尔质量的2.0%。
进一步地,有机溶剂为10wt%的甲醇。
进一步地,步骤(1)中采用氙灯发射紫外光,其功率为300W。
本发明以浓度为10mg/L的罗丹明B溶液作为降解对象来测试本发明提供的Pt/Bi2WO6/CuS三元复合光催化剂的光催化性能。将0.1g本发明提供的所述光催化剂投入100mL罗丹明B溶液中,在黑暗条件下吸附30min后,将混合的反应液移入水冷反应槽中进行光催化反应,采用300W的氙灯为反应光源,并用滤光片滤去波长小于420nm的紫外光部分。每隔10min收集4mL罗丹明B反应液,利用滤纸实现固液分离,在554nm测量反应前后罗丹明B溶液的吸光度。测试结果表明,本发明提供的Pt/Bi2WO6/CuS三元复合光催化剂较单一的BWC4-1具有更好的可见光响应以及更优秀的光催化活性。详见具体实施部分与说明书附图。
本发明通过紫外光原位还原法将Pt单质负载在BWC4-1光催化剂表面得到Pt/Bi2WO6/CuS三元复合光催化剂,即可在不需要表面活性剂和复杂的工艺的条件下无污染制备出Pt/Bi2WO6/CuS三元复合光催化剂,在不需要表面活性剂和复杂的工艺的条件下无污染制备出纳米微球结构的Pt/Bi2WO6/CuS三元复合光催化剂。
本发明的有益效果为:
1)本发明所用原料均为常用化学试剂,且来源广泛,价廉易得;
2)本发明提供的催化剂在制备过程中未引入有毒有害的表面活性剂;
3)本发明制备工艺简单、对设备的要求较低,过程简易反应条件可控性强;
4)本发明制备的Pt/Bi2WO6/CuS三元复合光催化剂较单一BWC4-1在光催化反应中对可见光具有更好的响应具有更优秀的光催化活性。
附图说明
图1为Pt/Bi2WO6/CuS三元复合光催化剂的XRD图;
图2为不同Pt负载量的Pt/BWC4-1光催化剂与BWC4-1的光催化活性图;
图3为Pt/Bi2WO6/CuS三元复合光催化剂在氙灯下光催化降解罗丹明B溶液(20mg/L)活性图。
具体实施方式
下面对本发明的具体实施方式进行描述,以便于本技术领域的技术人员理解本发明,但应该清楚,本发明不限于具体实施方式的范围,对本技术领域的普通技术人员来讲,只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内,这些变化是显而易见的,一切利用本发明构思的发明创造均在保护之列。
实施例1
在烧杯中倒入提前制备好的10%的甲醇溶液50mL,再加入制备好的BWC4-1样品进行搅拌,边搅边滴入能析出与BWC4-1摩尔百分比为0.5%的氯铂酸,然后将烧杯转移到氙灯系统下,在紫外光照射下搅拌90分钟后。搅拌完成后,倒掉上清液,剩下的沉淀分别用去离子水和无水乙醇洗涤三次,将清洗过的样品放入80℃恒温鼓风干燥箱中至完全风干。
实施例2
在烧杯中倒入提前制备好的10%的甲醇溶液50mL,再加入制备好的BWC4-1样品进行搅拌,边搅边滴入能析出与BWC4-1摩尔百分比为1%的氯铂酸,然后将烧杯转移到氙灯系统下,在紫外光照射下搅拌90分钟后。搅拌完成后,倒掉上清液,剩下的沉淀分别用去离子水和无水乙醇洗涤三次,将清洗过的样品放入80℃恒温鼓风干燥箱中至完全风干。
实施例3
在烧杯中倒入提前制备好的10%的甲醇溶液50mL,再加入制备好的BWC4-1样品进行搅拌,边搅边滴入能析出与BWC4-1摩尔百分比为1.5%的氯铂酸,然后将烧杯转移到氙灯系统下,在紫外光照射下搅拌90分钟后。搅拌完成后,倒掉上清液,剩下的沉淀分别用去离子水和无水乙醇洗涤三次,将清洗过的样品放入80℃恒温鼓风干燥箱中至完全风干。
实施例4
在烧杯中倒入提前制备好的10%的甲醇溶液50mL,再加入制备好的BWC4-1样品进行搅拌,边搅边滴入能析出与BWC4-1摩尔百分比为2%的氯铂酸,然后将烧杯转移到氙灯系统下,在紫外光照射下搅拌90分钟后。搅拌完成后,倒掉上清液,剩下的沉淀分别用去离子水和无水乙醇洗涤三次,将清洗过的样品放入80℃恒温鼓风干燥箱中至完全风干。
实施例5
在烧杯中倒入提前制备好的10%的甲醇溶液50mL,再加入制备好的BWC4-1样品进行搅拌,边搅边滴入能析出与BWC4-1摩尔百分比为2.5%的氯铂酸,然后将烧杯转移到氙灯系统下,在紫外光照射下搅拌90分钟后。搅拌完成后,倒掉上清液,剩下的沉淀分别用去离子水和无水乙醇洗涤三次,将清洗过的样品放入80℃恒温鼓风干燥箱中至完全风干。
对比例1
通过溶剂热法由Bi2WO6粉末与CuS的前驱体醋酸铜和硫脲反应而得到的。首先,将0.05g醋酸铜和0.076g硫脲分别溶解在40mL乙二醇中。充分搅拌10分钟后,将溶解了硫脲的乙二醇溶液缓慢滴入溶解有醋酸铜的乙二醇溶液中并保持搅拌。然后,将0.698g制备好的Bi2WO6粉末添加到该混合溶液中,继续搅拌。搅拌过程中滴入稀硝酸溶液将混合溶液的pH值调节至4。充分搅拌30分钟后,将所得混合物转移至100mL的具有聚四氟乙烯内村的高压反应釜中,将高压反应釜放入150℃恒温真空干燥箱中反应12小时后取出降温。待高温反应釜冷却至室温之后,开启高温反应釜取出内胆倒掉上清液将剩下的混合液置于离心管中进行离心分离,分别用去离子水和无水乙醇洗涤三次,将清洗过的沉淀放入80℃恒温鼓风干燥箱中至完全风干。获得了Bi2WO6与CuS摩尔质量比为4:1的Bi2WO6/CuS复合光催化剂样品,将其命名为BWC4-1。
试验例
1、X射线衍射图谱检测
图1为实施例4制得的2%Pt/BWC4-1三元光催化剂样品的X射线衍射图谱,如图示,2%Pt/BWC4-1光催化剂的所有衍射峰都与BWC4-1一一对应,没有观察到其他杂质峰且强度几乎一致,表明在该的实验条件下制备的三元复合光催化剂样品结晶度很好。图中无法观察到Pt单质的衍射峰,但是掺杂了Pt的BWC4-1样品光催化剂活性有明显的提高,说明Pt单质成功负载在了BWC4-1表面形成了光催化活性点位,但是由于Pt负载的量极少,都高度分散在BWC4-1催化剂的表面,所以无法检测到Pt单质的衍射峰。
2、光催化降解
从图2中可以看出所有负载了Pt的BWC4-1样品对罗丹明B的光催化降解效率都得到了提升,当Pt的负载量从0.5%到2%时,Pt/Bi2WO6/CuS三元光催化剂对罗丹明B的降解速率与Pt的负载量是呈正比关系,Pt负载的量越多Pt/Bi2WO6/CuS对罗丹明B的降解速率逐渐提高,当Pt的负载量为2%时Pt/Bi2WO6/CuS光催化活性最高,能在40分钟的时候将溶液中罗丹明B分子完全降解,降解速率是BWC4-1样品的1.5倍。当Pt的负载量增加到6%时,Pt/Bi2WO6/CuS光催化剂的光催化活性突然下降,对罗丹明B的降解效率比BWC4-1略微低一点,导致上述现象的原因可能是在BWC4-1表面负载了Pt单质之后,Pt可以作为光催化剂中的电子陷阱,使得受到光激发产生的光生电子与空穴复合的几率降低,因此Pt负载的量越多,电子陷阱就越多,使得Pt/Bi2WO6/CuS光催化剂的光催化活性越高,但是当Pt的负载量进一步增加之后,分散在催化剂表面的Pt原子簇会越来聚集以至于发生团聚现象,反而会成为光生载流子的复合中心,大大增加了光生载流子的复合概率,导致催化剂的光催化活性不升反降。
图3展示的是在可见光条件下,2%Pt/BWC4-1三元复合光催化剂与BWC4-1光催化剂的光催化性能比较,可以明显观察到BWC4-1负载了Pt之后光催化降解罗丹明B效率得到了提高,说明Pt单质的负载可以显着改善BWC4-1催化剂对可见光的响应范围,使其对光的响应范围向可见光区域发生红移,让复合光催化剂在可见光下也能有相对优秀的光催化活性。
Claims (8)
1.一种Pt/Bi2WO6/CuS三元复合光催化剂,其特征在于,所述三元复合光催化剂中的Pt弥散分布在Bi2WO6/CuS纳米微球的表面,并使两相界面之间形成异质结结构;所述Pt为Bi2WO6/CuS纳米微球的摩尔质量的0.5~2.5%。
2.根据权利要求1所述的Pt/Bi2WO6/CuS三元复合光催化剂,其特征在于,所述Pt与Bi2WO6和/或CuS之间形成异质结。
3.根据权利要求1所述的Pt/Bi2WO6/CuS三元复合光催化剂,其特征在于,所述Pt为Bi2WO6/CuS纳米微球的摩尔质量的2.0%。
4.根据权利要求1所述的Pt/Bi2WO6/CuS三元复合光催化剂,其特征在于,所述Bi2WO6/CuS纳米微球中Bi2WO6和CuS的摩尔质量比为4:1。
5.一种权利要求1~4任一项所述的三元复合光催化剂的制备方法,其特征在于,包括以下步骤:
(1)用有机溶剂溶解Bi2WO6/CuS纳米微球,然后在搅拌的过程中加入氯铂酸,再将其置于功率为250~400W的紫外光下搅拌反应90~120min;所述氯铂酸析出的铂单质为Bi2WO6/CuS纳米微球摩尔质量的0.5~2.5%;
(2)反应完成后过滤并收集洗涤固相产物,再于80~120℃风干,得该三元复合光催化剂。
6.根据权利要求5所述的制备方法,其特征在于,所述氯铂酸析出的铂单质为Bi2WO6/CuS纳米微球摩尔质量的2.0%。
7.根据权利要求5所述的制备方法,其特征在于,所述有机溶剂为10wt%的甲醇。
8.根据权利要求5所述的制备方法,其特征在于,所述紫外光的功率为300w。
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