CN109433185A - 一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂 - Google Patents
一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 13
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 9
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 8
- DPSWNBLFKLUQTP-UHFFFAOYSA-N bismuth vanadium Chemical compound [V].[Bi] DPSWNBLFKLUQTP-UHFFFAOYSA-N 0.000 title claims abstract description 7
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 7
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 title claims abstract description 7
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- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 12
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
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- 239000000243 solution Substances 0.000 claims abstract description 7
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- 238000005406 washing Methods 0.000 claims abstract description 7
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- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
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- 229910000831 Steel Inorganic materials 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
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- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract 1
- -1 indium nitrate bismuth nitrate Chemical compound 0.000 abstract 1
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- 238000007146 photocatalysis Methods 0.000 description 9
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
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- SRNMFPSMASDEKJ-UHFFFAOYSA-N indium;nitric acid Chemical compound [In].O[N+]([O-])=O SRNMFPSMASDEKJ-UHFFFAOYSA-N 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical group [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂,将偏钒酸铵加入蒸馏水中,摩尔比为1:4的硝酸铟和硝酸铋加入2mol/L的硝酸中,搅拌3h,然后在搅拌下将硝酸铟硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3小时,用氨水调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中,充填度约为70%,于150℃加热24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得InVO4/单斜BiVO4/四方BiVO4复合材料。此方法简单易行,可重复性高。可按比例扩大批量生产;在低维纳米材料的制备及应用方面有广阔的前景。
Description
技术领域
本发明属于纳米材料制备的技术领域,特别涉及一种一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂。
背景技术
近年来,环境污染和能源危机是人们面临和亟待解决的重要课题。半导体光催化技术由于其反应彻底、反应条件温和、无二次污染等优点,在环境污染治理方面显现出巨大的应用前景。目前,以TiO2为主的半导体光催化剂由于其电子空穴对复合率高与太阳能利用率低等缺点,使其在实际应用上面临着很大的挑战。因此,在对TiO2进行改性研究的同时,研究开发新型高效的光催化材料也成为了一个重要的研究方向。
钒酸铋(BiVO4)具有带隙窄、无毒、稳定性高等优点,但是由于电子-空穴对复合率高而影响了其光催化效率。半导体BiVO4主要有三种晶体结构,分别为四方白钨矿结构、单斜白钨矿结构和四方锆石结构。结构决定性质,不同晶相的BiVO4光催化性能不同。InVO4作为另一种重要的基础半导体光催化剂,也受到了广泛的关注。现在更需要一种将BiVO4和InVO4结合,而且光催化性能好的光催化剂。
发明内容
本发明的目的是要提供一种一步水热技术制备InVO4/同质异相结BiVO4光催化剂的方法,InVO4与BiVO4同质异相结形成三元复合结构,使得光生电子-空穴对的复合率降低,有利于提高催化剂的光催化性能。
本发明的技术方案是:
一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂,将偏钒酸铵加入蒸馏水中,摩尔比为1:4的硝酸铟和硝酸铋加入2mol/L的硝酸中,搅拌3h,然后在搅拌下将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用浓度为1mol·L-1的氨水调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中进行水热反应,水热反应条件是充填度约为70%,水热反应温度为150℃,水热反应时间为24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
0.5-1mmol偏钒酸铵加入12-24ml蒸馏水中,0.1-0.2mmol硝酸铟和0.2-0.8mmol硝酸铋加入3-6ml硝酸(2mol/L)中,分别搅拌3小时,将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用氨水(1mol·L-1)调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中,充填度约为70%,于150℃加热24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
本发明的有益效果是:
1、本发明要解决的技术问题是,公开一种制备InVO4/同质异相结BiVO4三元复合光催化剂的一步水热方法,不需要复杂昂贵的设备,合成条件温和,成本低,催化剂稳定性好,具有较大的应用潜力。
2、本发明的整个工艺过程简单易控制,可重复性高,具有很高的实用价值和应用前景。
3、本发明首次采用一步水热技术制备InVO4/单斜BiVO4/四方BiVO4三元复合光催化剂,所制备的复合催化剂通过半导体异质结、半导体同质异相结协同作用有效地提高体系的光生载流子的分离效率,从而提高可见光光催化活性。
4、所制备的InVO4/单斜BiVO4/四方BiVO4三元复合光催化剂在可见光照射下(λ>420nm),光催化性能较纯相BiVO4、InVO4及InVO4/BiVO4二元复合材料有显著提高。
附图说明
图1为所制备的InVO4/单斜BiVO4/四方BiVO4复合材料的XRD图。从中可以观察到InVO4(JCPDS No.48-0898)、单斜结构BiVO4(JCPDS No.14-0688)、四方结构BiVO4(JCPDSNo.14-0133)。说明所制备样品为InVO4/单斜BiVO4/四方BiVO4三元复合物。图中没有观察到任何杂相的衍射峰,且衍射峰尖锐,说明样品结晶度较高。
图2所制备的InVO4/单斜BiVO4/四方BiVO4的SEM图(a)及相对应的EDS元素分布图:(b)O K,(c)In L,(d)Bi M。
从图2a中可以看到所制备的样品为球形。从图2a中还可以观察到少量线状InVO4沉积在微米球的表面。EDS元素分布图说明复合物中含有In、Bi、V、O四种元素,再一次证明了复合物为InVO4/异相结BiVO4复合物。
图3所制备光催化剂可见光(λ>420nm)降解罗丹明曲线从中可以观察到所制备的InVO4/单斜BiVO4/四方BiVO4三元复合光催化剂在可见光照射下,光催化性能较纯相BiVO4、InVO4及InVO4/BiVO4二元复合材料有显著提高。
具体实施方式:
实施例一1mmol偏钒酸铵加入24ml蒸馏水中,0.2mmol硝酸铟和0.8mmol硝酸铋加入6ml硝酸(2mol/L)中,分别搅拌3小时,将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用氨水(1mol·L-1)调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中,充填度约为70%,于150℃加热24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
实施例二0.5mmol偏钒酸铵加入12mL蒸馏水中,0.1mmol硝酸铟和0.4mmol硝酸铋加入3ml硝酸(2mol/L)中,分别搅拌3小时,将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用氨水(1mol·L-1)调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中,充填度约为70%,于150℃加热24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
本发明首次在不同相的BiVO4中构建同质异相结,晶格高度匹配,并用一步水热法制备InVO4修饰同质异相结BiVO4光催化剂,实现了光生载流子的高效分离,从而提高催化剂可见光催化性能。InVO4与BiVO4同质异相结形成三元复合结构,使得光生电子-空穴对的复合率降低,有利于提高催化剂的光催化性能。
Claims (2)
1.一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂,其特征在于:将偏钒酸铵加入蒸馏水中,摩尔比为1:4的硝酸铟和硝酸铋加入2mol/L的硝酸中,搅拌3h,然后在搅拌下将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用浓度为1mol·L-1的氨水调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中进行水热反应,水热反应条件是充填度约为70%,水热反应温度为150℃,水热反应时间为24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
2.根据权利要求1所述的一步水热法制备钒酸铟/同质异相结钒酸铋复合光催化剂,其特征在于:
0.5-1mmol偏钒酸铵加入12-24ml蒸馏水中,0.1-0.2mmol硝酸铟和0.2-0.8mmol硝酸铋加入3-6ml硝酸(2mol/L)中,分别搅拌3小时,将硝酸铟、硝酸铋混合溶液滴入偏钒酸铵水溶液中,此时悬浊液呈黄色,再搅拌3h,用氨水(1mol·L-1)调节溶液pH等于3,再搅拌30min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中,充填度约为70%,于150℃加热24h。反应结束后,将此悬浊液用去离子水和无水乙醇洗涤3次,将洗涤后的沉淀放入干燥箱50℃烘干,得到黄色粉末,即为InVO4/单斜BiVO4/四方BiVO4复合材料。
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