CN109675547A - 一种中空立方体型锡酸锌光催化剂的制备方法及其应用 - Google Patents
一种中空立方体型锡酸锌光催化剂的制备方法及其应用 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 13
- 238000003760 magnetic stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 239000011592 zinc chloride Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 5
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910007694 ZnSnO3 Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910007717 ZnSnO Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
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Abstract
本发明公开了一种中空立方体型锡酸锌光催化剂的制备方法及其应用,采用共沉淀法合成具有中空立方体结构的锡酸锌光催化剂,最终获得高活性的可见光催化剂,该光催化剂具有在模拟太阳光照射下高效降解有机污染物的特性,对于拓展纳米光催化技术降解废水污染物的工业化应用范围、节省废水处理能耗,具有重大的现实意义。
Description
技术领域
本发明属于光催化材料的合成技术领域,具体涉及一种中空立方体型锡酸锌光催化剂的制备方法及其应用。
背景技术
近年来,光催化技术以其高效节能、无二次污染、适用范围广等优点在难生物降解有机废水处理中表现出良好的应用前景。它能够在温和条件下有效地将大分子转化为小分子,因此可用于净化工业废水,将水分解为氢气和氧气以获得清洁的可再生能源。TiO2是研究最多的光催化剂,但是它的量子产率低,太阳能利用率低,这极大地限制了其应用范围。因此,开发出具有环保性和高效可见光催化活性的新型光催化剂已成为光催化研究的热点。
n-型半导体ZnSnO3由于其高电子迁移率和高导电性,在光催化、光电器件和电池功能涂层等方面具有潜在的应用。大量研究表明,不同的合成方法不仅影响ZnSnO3的颗粒大小、形状及其晶型等形态结构特征,还会影响其光学性质及其催化活性。ZnSnO3有多种合成方法,例如:热蒸发、共沉淀法和水热合成等。其中,共沉淀法具有合成简单、能耗低等优点,具有极大的工业化应用前景。中空结构往往比相同粒径的颗粒具有更大的比表面积和渗透性能,因而具有更好的吸附性能和光催化活性。采用共沉淀法合成具有中空立方体结构的ZnSnO3有望获得高活性的可见光催化剂,对于拓展纳米光催化技术降解废水污染物的工业化应用范围、节省废水处理能耗,具有重大的现实意义。
发明内容
本发明解决的技术问题是提供了一种工艺简单且成本低廉的中空立方体型锡酸锌光催化剂的制备方法,该方法制得的光催化剂具有在模拟太阳光照射下高效降解有机污染物的特性。
本发明为解决上述技术问题采用如下技术方案,一种中空立方体型锡酸锌光催化剂的制备方法,其特征在于具体步骤为:将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为0.41-1.67mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂。
本发明所述的中空立方体型锡酸锌光催化剂在太阳光照射下高效降解有机污染物中的应用,其特征在于具体过程为:将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为0.41mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂,该锡酸锌光催化剂经过模拟太阳光照射120min,对10mg/L的亚甲基蓝废水的去除率为98%。
本发明与现有技术相比具有以下有益效果:本发明采用简单的化学沉淀法制备出具有中空立方体型锡酸锌光催化剂,制得的光催化剂具有在模拟太阳光照射下高效降解有机污染物的特性。
附图说明
图1是实施例3制得的中空立方体型锡酸锌光催化剂的XRD图;
图2是实施例3制得的中空立方体型锡酸锌光催化剂的SEM图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为1.67mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂,该锡酸锌光催化剂经过模拟太阳光照射120min,对10mg/L的亚甲基蓝废水的去除率为34.37%。
实施例2
将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为1mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂,该锡酸锌光催化剂经过模拟太阳光照射120min,对10mg/L的亚甲基蓝废水的去除率为46.28%。
实施例3
将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为0.41mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂,该锡酸锌光催化剂经过模拟太阳光照射120min,对10mg/L的亚甲基蓝废水的去除率为98%。
基于以上实施例,选取NaOH溶液的摩尔浓度为0.41mol/L制备的锡酸锌光催化剂的性能较优,通过进一步的表征研究,该条件下制备的锡酸锌光催化剂具有中空立方体结构,相比于传统的光催化材料,本发明制得的锡酸锌光催化剂能够响应自然太阳光,具有可见光催化活性,且制备方法简单快速,无二次污染。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (2)
1. 一种中空立方体型锡酸锌光催化剂的制备方法,其特征在于具体步骤为:将1.363gZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为0.41-1.67mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂。
2.根据权利要求1所述的方法制得的中空立方体型锡酸锌光催化剂在太阳光照射下高效降解有机污染物中的应用,其特征在于具体过程为:将1.363g ZnCl2溶于100mL水中,在磁力搅拌器上搅拌混合均匀后加入2.941g柠檬酸钠,继续搅拌30min得到溶液A;再称取3.506g SnCl4·5H2O溶于50mL乙醇溶液,在磁力搅拌器上搅拌溶解完全后得到溶液B,将溶液B与溶液A混合后在搅拌条件下反应30min,然后逐滴滴加25mL摩尔浓度为0.41mol/L的NaOH溶液,溶液逐渐浑浊,反应15min后将沉淀物离心、水洗后置于干燥箱中烘干,再置于研钵中研磨得到前驱体物质,将前驱体物质置于管式炉中于300℃煅烧3h得到中空立方体型锡酸锌光催化剂,该锡酸锌光催化剂经过模拟太阳光照射120min,对10mg/L的亚甲基蓝废水的去除率为98%。
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