CN108906032B - 一种GOQDs/TiO2/WO3光催化剂的制备及其应用 - Google Patents
一种GOQDs/TiO2/WO3光催化剂的制备及其应用 Download PDFInfo
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Abstract
本发明涉及的是一种GOQDs/TiO2/WO3光催化剂的制备及其应用。该材料以三氧化钨(WO3)纳米片为基底材料,且氧化石墨烯量子点(GOQDs)和二氧化钛(TiO2)均匀的负载在WO3纳米片上,制备方法为首先用水热法将氧化石墨烯制备成尺寸大小均匀的GOQDs,然后采用一步水热法合成GOQDs/TiO2/WO3三元异质结光催化剂材料,提高了TiO2的光量子产率、拓展了光吸收波长、提高了光催化反应的活性。然后以汞灯为紫外光源,以反渗透浓水为原水,以重金属类内分泌干扰物为目标污染物进行光催化工艺处理,通过火焰原子吸收分光光度法对结果进行监测。本发明制备的光催化剂活性较高,拓宽了光催化技术在污水处理中的应用,为去除废水中重金属类内分泌干扰物提供强有力的支撑。
Description
技术领域
本发明属于光催化材料、水处理技术领域,涉及到光催化剂GOQDs/TiO2/WO3的制备及其在废水处理中的应用。
背景技术
反渗透技术在污水处理行业中的应用愈加广泛,反渗透浓水的处理和排放也引起了人们的关注。其中反渗透浓水中的重金属类内分泌干扰物属于新型污染物,浓度较低却对人体和生态系统产生严重影响,威胁了生物和人类的健康,因此,去除反渗透浓水中的重金属类内分泌干扰物具有十分重要的现实意义。
吸附法和膜分离法是处理重金属类内分泌干扰物常用方法,在应用的过程中起到了一定的富集作用但是重金属价态未发生改变,没有达到消除毒性的目的。光催化法是近年来发展起来的新型技术,改变了重金属类内分泌干扰物的形态且能够在常温常压下反应,在处理反渗透浓水中的重金属类内分泌干扰物显示出独特的优势(魏添昱, 陈荣, 马田,等. 光催化应用于处理水中重金属离子的研究进展[J]. 江西化工, 2015(5):13-17.)。二氧化钛(TiO2)是目前研究和应用中最广泛的半导体材料,然而传统的TiO2光催化剂存在两大主要缺陷:光生载流子极易复合及较宽的带隙(3.2ev),为解决上述两个问题,本专利将WO3和TiO2复合,形成TiO2/WO3半导体异质结能够有效提高电荷分离效率,还可以将光响应扩展到可见光区;另外GOQDs的量子尺寸效应、量子限域效应和表面效应能够增强光生电子-空穴的分离,进一步提高TiO2活性。
发明内容
本发明提供了一种能够高效去除反渗透浓水中重金属类内分泌干扰物的工艺,无需预处理,光催化方法简单安全,操作简易。通过一步水热法合成GOQDs/TiO2/WO3催化剂,此催化剂具有较高的电子传输能力,加强了光生电子还原重金属离子作用,由于光生空穴的氧化性,反渗透浓水中的有机污染物可以同时去除。
本发明的技术方案是:(一)通过一步水热法合成GOQDs/TiO2/WO3光催化剂,该催化剂以WO3纳米片为基底材料,TiO2和GOQDS均匀的负载在WO3纳米片上,WO3纳米片直径在100nm左右为正交晶型,TiO2直径在40nm左右为锐钛矿型,GOQDs直径在6nm以下;(二)以GOQDs/TiO2/WO3三元异质结纳米复合材料为光催化剂进行光催化反应,还原反渗透浓水中的重金属类内分泌干扰物。
具体步骤如下:
(1)GOQDs/TiO2/WO3光催化剂的制备:取20~50ml的GOQDs溶液超声并加入0.00075~0.001mol的Na2WO4•2H2O,剧烈搅拌1 h左右,使Na2WO4•2H2O全部溶解;将80ml的无水乙醇放在磁力搅拌仪上面,边搅拌边滴加1~2ml的钛酸丁酯,并加入0.4ml的HF,搅拌30min;将这两种溶液混合并搅拌1~2h后转移至100ml的水热高压反应釜中进行水热反应(反应温度为160℃~180℃,反应时间为18h~24h),将所得产品用纯水和无水乙醇洗涤多次至中性,然后在60℃下于恒温干燥箱中干燥,得到GOQDs/TiO2/WO3光催化剂材料。
(2)由上述制备方法制备的GOQDs/TiO2/WO3光催化剂在废水处理中的应用:以反渗透浓水为处理原水,以重金属类内分泌干扰物为目标污染物,加入GOQDs/TiO2/WO3三元异质结光催化剂,光催化剂在反渗透浓水中的浓度为0.2~0.8mg/l,首先进行0.5~1.5h的暗反应,然后在紫外灯的照射下进行20min~2h的光催化反应以去除反渗透浓水中的重金属离子。
本发明的特点及有益效果是:
1.利用简单的水热法合成了GOQDs,大小均匀,大部分在4-6nm之间,具有-COOH等含氧官能团,增加了复合材料的水溶性,其显著的边缘效应和量子限域效应有利于降低光生载流子的复合率,实现了光生电子-空穴对的分离,促进了重金属类内分泌干扰物的去除。
2.通过一步水热法合成了GOQDs/TiO2/WO3光催化剂,反应过程简单易控制,异质结催化剂体系有利于光生电子的迁移,使光生电子和空穴对发挥还原氧化作用,降低了TiO2的禁带宽度,实现了可见光响应,合成的复合材料的光催化活性较高。
3.本发明采用的方法安全,流程简单,能够减少对水体环境的危害,加快了光催化技术在处理反渗透浓水中的应用,为去除废水中较低浓度的重金属类内分泌干扰物提供了优选工艺。
附图说明
图1.GOQDs/TiO2/WO3光催化剂的透射电镜图片:(a)氧化石墨烯量子点,(b)三氧化钨,(c)、(d)GOQDs/TiO2/WO3光催化剂。
具体实施方式
下面结合具体实施案例对本发明作进一步解释,所处理的反渗透浓水来自齐鲁石化公司炼化废水,其中Cd2+浓度为0.386mg/l,Pb2+浓度为0.351mg/l。
实施例1
取30ml的GOQDs溶液超声并加入0.3771g的Na2WO4•2H2O,剧烈搅拌1h左右,使Na2WO4•2H2O全部溶解;将80ml的无水乙醇放在磁力搅拌仪上面,边搅拌边滴加1ml钛酸丁酯,并加入0.4ml的HF,搅拌30min;将这两种溶液混合并搅拌1~2h后转移至100ml的水热高压反应釜中进行水热反应(160℃,24h),将所得产品用纯水和无水乙醇洗涤多次至中性,然后在60℃下于恒温干燥箱中干燥,得到GOQDs/TiO2/WO3光催化剂材料。
取80ml的反渗透浓水进行光催化反应,调节其pH为6并加入35.2mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照80min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.028mg/l,C(Cd2+)=0.135 mg/l,Pb2+的去除率为:91.84%,Cd2+的去除率为:64.91%。
实施例2
GOQDs/TiO2/WO3光催化剂材料制备方法如实施例1。
取80ml的反渗透浓水进行光催化反应,调节其pH为7并加入41.6mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照60min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.007 mg/l,C(Cd2+)=0.132 mg/l,Pb2+的去除率为:97.96%,Cd2+的去除率为:65.85%。
实施例3
GOQDs/TiO2/WO3光催化剂材料制备方法如实施例1。
取80ml的反渗透浓水进行光催化反应,调节其pH为4并加入48.0mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照40min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.007 mg/l,C(Cd2+)=0.124 mg/l,Pb2+的去除率为:97.96%,Cd2+的去除率为:67.73%。
实施例4
GOQDs/TiO2/WO3光催化剂材料制备方法如实施例1。
取80ml的反渗透浓水进行光催化反应,调节其pH为5并加入54.0mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照20min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.003 mg/l,C(Cd2+)=0.153 mg/l,Pb2+的去除率为:98.98%,Cd2+的去除率为:60.20%。
实施例5
取30ml的GOQDs溶液超声并加入0.4948gNa2WO4•2H2O,剧烈搅拌1h左右,使Na2WO4•2H2O全部溶解;将80ml的无水乙醇放在磁力搅拌仪上面,边搅拌边滴加1ml钛酸丁酯,并加入0.4ml的HF,搅拌30min;将这两种溶液混合并搅拌1~2h后转移至100ml的水热高压反应釜中进行水热反应(160℃,24h),将所得产品用纯水和无水乙醇洗涤多次至中性,然后在60℃下于恒温干燥箱中干燥,得到GOQDs/TiO2/WO3光催化剂材料。
取80ml的反渗透浓水进行光催化反应,调节其pH为7并加入35.2mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照40min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.100mg/l,C(Cd2+)=0.128mg/l,Pb2+的去除率为:71.43%,Cd2+的去除率为:66.79%。
实施例6
GOQDs/TiO2/WO3光催化剂材料制备方法如实施例5。
取80ml的反渗透浓水进行光催化反应,调节其pH为6并加入41.6mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照20min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.136 mg/l,C(Cd2+)=0.128 mg/l,Pb2+的去除率为:61.22%,Cd2+的去除率为:66.79%。
实施例7
GOQDs/TiO2/WO3光催化剂材料制备方法如实施例5。
取80ml的反渗透浓水进行光催化反应,调节其pH为5并加入48.0mg的GOQDs/TiO2/WO3光催化剂,避光搅拌30min后转入光催化反应装置,光照80min后测定反渗透浓水中的Cd2 +和Pb2+浓度,经测定,C(Pb2+)=0.100mg/l,C(Cd2+)=0.132 mg/l,Pb2+的去除率为:71.43%,Cd2+的去除率为:65.85%。
Claims (4)
1.一种GOQDs/TiO2/WO3光催化剂的制备方法,其特征在于,具体步骤如下:
(1)取20~50 ml的氧化石墨烯量子点GOQDs溶液超声并加入钨酸钠Na2WO4•2H2O,剧烈搅拌1 h左右,使Na2WO4•2H2O全部溶解;
(2)将80 ml的无水乙醇放在磁力搅拌仪上面,边搅拌边滴加钛酸丁酯,并加入0.4 ml的HF,搅拌30 min;
(3)将这两种溶液混合并搅拌1~2 h后转移至100 ml的水热高压反应釜中进行水热反应,水热处理的反应温度在160~180℃,反应时间为18~24 h,反应结束后将所得产品用纯水和无水乙醇洗涤多次至中性,然后在60℃下于恒温干燥箱中干燥,得到GOQDs/TiO2/WO3光催化剂。
2.按权利要求1所述的GOQDs/TiO2/WO3光催化剂的制备方法,其特征在于,步骤(1)中Na2WO4•2H2O物质的量为0.00075~0.001 mol,步骤(2)中钛酸丁酯的体积为1~2 ml。
3.按权利要求1所述的GOQDs/TiO2/WO3光催化剂的制备方法,其特征在于,步骤(3)制备的GOQDs/TiO2/WO3光催化剂中元素占比为:Ti:30~40%,W:30~40%,C:10~20%,O:10~20%。
4.由权利要求1~3中任一项所述的制备方法制备的GOQDs/TiO2/WO3作为光催化剂在废水处理中的应用。
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