CN108421553A - 一种钒酸铈改性二硒化钼复合光催化剂的制备 - Google Patents
一种钒酸铈改性二硒化钼复合光催化剂的制备 Download PDFInfo
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 42
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 41
- 239000011733 molybdenum Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 title claims abstract description 35
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- 235000016768 molybdenum Nutrition 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
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- 239000011669 selenium Substances 0.000 claims 3
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- 238000007146 photocatalysis Methods 0.000 abstract description 9
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- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 17
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical group [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 7
- 229940012189 methyl orange Drugs 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 229910015667 MoO4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
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- 230000006798 recombination Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000004134 energy conservation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Abstract
本发明公开了一种钒酸铈改性二硒化钼复合光催化剂的制备方法及其在环境污染物治理领域的应用,属于材料制备及光催化研究领域。该催化剂的特点有:具有维的形貌特征,由2维结构的二硒化钼片与钒酸铈纳米粒子复合而成。在制备光催化剂过程中,采用工艺简单的水热法合成出钒酸铈改性二硒化钼复合光催化剂。在钒酸铈的作用下,钒酸铈改性二硒化钼复合光催化剂表现出高的光催化性能,促进了二硒化钼光催化剂的应用。
Description
技术领域
本发明属于材料的合成和光催化技术领域,主要涉及一种钒酸铈改性二硒化钼复合光催化剂的制备及其光催化活性的研究。
背景技术
随着人们环境保护意识的增强,水污染的问题已受到越来越多的关注。传统的污水处理方法已经满足不了人们的要求。寻找出一种清洁,高效,节能环保的污水处理方法,成了人们研究的热点方向。
自1972年首次发现TiO2具有光催化活性以来,光催化技术的研究一直是材料领域的热点方向。光催化技术凭借其节能环保、无二次污染等优点为污水的处理提供了一个非常好的解决途径。半导体光催化材料可以利用取之不尽、用之不竭的太阳能处理空气中或者水中有毒有害物质,改善环境,达到资源利用生态化的目的。目前,各种不同的半导体光光催化剂材料被广泛研究,如ZnO,g-C3N4等,但是二硒化钼凭借其材料来源广泛,价格低廉,高的吸附性能等优点成为光催化研究的主要材料,并且开发出多种产品应用于实际生活中。
但是, 二硒化钼光催化剂也存在着一些缺陷,例如,其太阳光利用率低;对降解底物的吸附性能差;量子效率偏低,并且具有高得光生电子-空穴复合速率,这些缺陷都阻碍了其实际应用。在这种背景下,如何提高二硒化钼的光催化效率和拓宽其光相应范围,成了二硒化钼光催化剂的研究重点。至今为止,各种方法已经被用来提高其量子效率和扩展其光相应范围,如:半导体复合化,形貌控制等。但是,上述方法改性后二硒化钼的光催化效率、稳定性以及在实际应用中的反复使用性受到了一定的限制。
近年来,钒酸铈由于具有高的光催化活性和合适的禁带宽度,吸引了人们的广泛注意。本发明利用钒酸铈作为改性剂,制备出钒酸铈改性二硒化钼复合光催化剂,形成2维结构,有效地提高了二硒化钼的可见光利用率和光催化活性。
发明内容
本发明的目的是制备出具有高的可见光利用率和高催化活性的二硒化钼基复合光催化剂,并且其催化循环稳定性高,推进二硒化钼的实际应用。
为实现本发明目的采用如下技术方案:
以钒酸铈作为改性剂,通过水热法,制备出钒酸铈改性二硒化钼复合光催化剂。在钒酸铈的作用下,提高二硒化钼的可见光催化活性。
一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征步骤如下:
(1)称取一定量Na2MoO4溶于50mL水中;
(2)称取一定量Se粉于上述溶液中,磁力搅拌均匀;
(3)称取0.2595g NaBH4溶于(2)溶液中,搅拌均匀;
(4)将步骤(3)溶液放入高压反应釜中,进行水热反应。将反应完全的样品离心洗涤,干燥后研磨即得到二硒化钼;
(5)称取0.5g二硒化钼,加入到50mL水中,加入适量硝酸铈到上述溶液,搅拌均匀;
(6)向步骤(5)溶液加适量钒酸铵,搅拌均匀;
(7)进行水热反应,产物经过离心洗涤,干燥后得到钒酸铈改性二硒化钼复合光催化剂。
步骤(1)中Na2MoO4质量为1.7g,浓度为34g/L。
步骤(2)中Se质量为1.6 g,浓度为32g/L。
步骤(4)中反应温度为200℃,反应时间为48h。
步骤(5)中硝酸铈的质量为0.1g,浓度为2g/L。
步骤(6)中钒酸铵0.03g,浓度为0.6g/L。
步骤(7)中水浴温度为180℃,时间15h。
步骤(7)中的离心清洗过程为先用乙醇清洗4次,再用去离子水清洗2次,离心速率10000rpm,时间6min。
所述钒酸铈改性二硒化钼复合光催化剂用于水溶液中有机污染物的可见光催化降解。
目标污染物为甲基橙。
本发明具有如下优点:
1.本发明采用水热法,制备出钒酸铈改性二硒化钼复合光催化剂的制备,属于新的复合体系。经扫描电镜可发现该材料是由钒酸铈纳米粒子附着在二硒化钼片表面复合而成(图1);
2.本发明中的钒酸铈改性二硒化钼复合光催化剂具有良好的光催化活性,其催化活性在二硒化钼的基础上有了显著的提升。在90min人造可见光源的照射下降解甲基橙染料,降解程度达到90%,是已报道的二硒化钼单体可见光催化活性的10倍 (图2)。
附图说明
图1为钒酸铈改性二硒化钼复合光催化剂的扫描电镜图。
图2为钒酸铈改性二硒化钼复合光催化剂的光催化降解图。
具体实施方式
一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征步骤如下:
(1)称取一定量Na2MoO4溶于50mL水中;
(2)称取一定量Se粉于上述溶液中,磁力搅拌均匀;
(3)称取0.2595gNaBH4溶于(2)溶液中,搅拌均匀;
(4)将步骤(3)溶液放入高压反应釜中,进行水热反应。将反应完全的样品离心洗涤,干燥后研磨即得到二硒化钼;
(5)称取0.5g二硒化钼,加入到50mL水中,加入适量硝酸铈到上述溶液,搅拌均匀;
(6)向步骤(5)溶液加适量钒酸铵,搅拌均匀;
(7)进行水热反应,产物经过离心洗涤,干燥后得到钒酸铈改性二硒化钼复合光催化剂。
步骤(1)中Na2MoO4质量为1.7g,浓度为34g/L。
步骤(2)中Se质量为1.6 g,浓度为32g/L。
步骤(4)中反应温度为200℃,反应时间为48h。
步骤(5)中硝酸铈的质量为0.1g,浓度为2g/L。
步骤(6)中钒酸铵0.03g,浓度为0.6g/L。
步骤(7)中水浴温度为180℃,时间15h。
步骤(7)中的离心清洗过程为先用乙醇清洗4次,再用去离子水清洗2次,离心速率10000rpm,时间6min。
所述钒酸铈改性二硒化钼复合光催化剂用于水溶液中有机污染物的可见光催化降解。
下面例举实施例子制备钒酸铈改性二硒化钼复合光催化剂。
实施案例1
一种钒酸铈改性二硒化钼复合光催化剂的制备。
称取Na2MoO41.7g,溶于50mL水溶液中,搅拌均匀;接着向溶液中加入1.6g Se粉,搅拌均匀;再加入NaBH4 0.2595g,搅拌均匀;将溶液放入反应釜中,进行水热反应,反应温度为200℃,反应时间为48h。反应完成后,离心洗涤,先用乙醇清洗4次,在用水洗2次,离心速度为10000rpm,时间为6min。最后烘箱中60℃干燥,研磨即得二硒化钼。
称取0.5g二硒化钼分散在50mL水中,加入0.1g硝酸铈,搅拌均匀;再加入0.03g钒酸铵,搅拌均匀后进行水热反应,水热温度为180℃,时间15h。产物经过离心洗涤,干燥后得到钒酸铈改性二硒化钼复合光催化剂。
实施案例2
钒酸铈改性二硒化钼复合光催化剂在可见光照射下降解甲基橙。
按实施案例1方法制得的钒酸铈改性二硒化钼复合光催化剂进行降解甲基橙实验。甲基橙溶液的浓度是1×10-5mol L-1;取复合材料粉体50mg,置于100mL上述甲基橙溶液中,在暗室中搅拌40分钟,然后将溶液置于紫外光被过滤掉的可见光源中,每10分钟取5mL甲基橙溶液,用紫外-可见分光光度计测出溶液中甲基橙的特征峰值。
按实施案例2得到钒酸铈改性二硒化钼复合光催化剂可见光降解甲基橙的降解曲线,见图2。从图2可以看出实施案例1制备的复合材料粉体在光照90min后催化降解达到90%,表现出高的可见光催化活性。
Claims (8)
1.一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征包括以下步骤:
(1)称取一定量Na2MoO4溶于50mL水中;
(2)称取一定量Se粉于上述溶液中,磁力搅拌均匀;
(3)称取0.2595gNaBH4溶于(2)溶液中,搅拌均匀;
(4)将步骤(3)溶液放入高压反应釜中,进行水热反应;将反应完全的样品离心洗涤,干燥后研磨即得到二硒化钼;
(5)称取0.5g二硒化钼,加入到50mL水中,加入适量硝酸铈到上述溶液,搅拌均匀;
(6)向步骤(5)溶液加适量钒酸铵,搅拌均匀;
(7)进行水热反应,产物经过离心洗涤,干燥后得到钒酸铈改性二硒化钼复合光催化剂。
2.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(1)Na2MoO4质量为1.7g,浓度为34g/L。
3.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(2)Se的质量为1.6,浓度为32g/Lg。
4.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(4)水热反应温度为200℃,反应时间为48h。
5.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(5)硝酸铈质量为0.1,浓度为2g/Lg。
6.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(6)钒酸铵质量为0.03,浓度为0.6g/Lg。
7.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于步骤(7)水热温度为180℃,时间15h。
8.根据权利要求1一种钒酸铈改性二硒化钼复合光催化剂的制备,其特征在于在二硒化钼片上生长钒酸铈纳米粒子,制备出钒酸铈改性二硒化钼复合光催化剂。
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