CN107930614B - 一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法 - Google Patents
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 10
- 229910052793 cadmium Inorganic materials 0.000 title claims description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 229910004575 Cd2Nb2O7 Inorganic materials 0.000 claims abstract description 18
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 15
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims abstract description 15
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000010955 niobium Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 230000005284 excitation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910003378 NaNbO3 Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012827 research and development Methods 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
- 238000000926 separation method Methods 0.000 description 1
- MUPJWXCPTRQOKY-UHFFFAOYSA-N sodium;niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Na+].[Nb+5] MUPJWXCPTRQOKY-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明涉及一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法,属于光催化材料领域。本发明采用水热法,以五氯化铌、硝酸镉、氢氧化钠为原料,在180‑240℃下水热处理36‑60小时,即可制备出Cd2Nb2O7/Cd(OH)2光催化材料,所制备材料具有优异的紫外光催化性能,在环境污水治理和能源领域具有广泛的应用前景。本发明所描述的制备方法相对简单,易于操作,不需要复杂设备。
Description
技术领域
本发明属于光催化材料水处理领域,尤其是涉及一种Cd2Nb2O7/Cd(OH)2光催化材料的制备。
背景技术
随着全球工农业的快速发展,日益恶化的环境问题越来越成为世界所关注的焦点,解决能源短缺和环境污染问题是实现可持续发展,对于实现人民对美好生活的追求异常重要。自从1972年Fujishima发现了TiO2半导体电极在紫外光照射下具有光解水的作用后,基于半导体材料的光催化技术作为一种新型绿色净化技术,能够直接吸收利用太阳光并将其转化为化学能,将水中有机污染物分解为水、二氧化碳或无毒小分子,具有成本低、高效稳定、无毒等优点,因此如何高效地利用太阳光进行光催化反应,亟待开发出更加高效的光催化剂。
由于Nb5+离子的d0电子组态,铌酸盐化合物在光催化领域表面出潜在的应用,如NaNbO3、SnNb2O6、Cd2Nb2O7。其中,Cd2Nb2O7具有立方晶体结构,空间群为Fd-3m,结构是由NbO6八面体网格和O-Cd-O链构成。Cd2Nb2O7除了具有特异的铁电性能,在紫外光激发下,还展现出优异的光催化性能。
本发明制备了一种Cd2Nb2O7/Cd(OH)2光催化材料,当该材料受到紫外光激发时,产生光电子空穴;同时利用Cd2Nb2O7和Cd(OH)2间构建的异质结,促进光生电子空穴的分离,从而获得高的光催化性能。该光催化材料制备方法仅是通过以五氯化铌、硝酸镉、氢氧化钠为原料,在180-240℃下水热处理36-60小时,即可一步得到性能优异的Cd2Nb2O7/Cd(OH)2光催化材料。
发明内容
本发明制备出了一种Cd2Nb2O7/Cd(OH)2光催化材料,该催化材料在紫外光激发下,可以快速降解水中有机污染物,在污水处理等领域有着广阔应用;该催化材料制备方法具有成本低、过程简单和易于操作的特点。
本发明涉及一种Cd2Nb2O7/Cd(OH)2光催化材料的制备,步骤如下:
(1)将适量的五氯化铌溶于25 mL无水乙醇中,搅拌得到澄清溶液,五氯化铌的摩尔浓度为0.1-0.2 mol/L;
(2)称量适量硝酸镉溶于25 mL去离子水中,搅拌得到澄清溶液,其中溶液中硝酸镉的摩尔浓度为五氯化铌的1.5-2.5倍;
(3)将以上两溶液混合搅拌,称取适量1.2-1.8 g NaOH溶于25 mL去离子水中后,加至混合液中,搅拌10分钟后装入水热釜中,在180-240℃下水热处理36-60小时,经洗涤干燥后即可得到Cd2Nb2O7/Cd(OH)2光催化材料。
该制备方法具有成本低、过程简单、易于操作的特点;所得Cd2Nb2O7/Cd(OH)2光催化材料在紫外光激发下,具有优异的光催化活性。
优选的,步骤(1)所得五氯化铌的摩尔浓度为0.16mol/L.
优选的,步骤(2)所得溶液中硝酸镉的摩尔浓度为五氯化铌的1.5倍。
优选的,步骤(3)在200℃下水热处理48小时。
本发明取得的优异效果是:
1. 该方法制得的Cd2Nb2O7/Cd(OH)2光催化材料在紫外光激发下,具有优异的光催化活性,在环境保护领域有着广阔应用前景;
2. 本发明所描述的制备过程具有成本低、过程简单、易于操作的特点。
附图说明
图1是实施例1Cd2Nb2O7/Cd(OH)2光催化材料的X射线衍射图谱;
图2是实施例1所得Cd2Nb2O7/Cd(OH)2光催化材料的扫描电子显微镜照片;
图3是实施例1制备的Cd2Nb2O7/Cd(OH)2光催化材料在紫外光激发下对罗丹明B的光催化降解效果图。
具体实施方式
下面通过具体实施方式对本发明作进一步说明,以帮助更好的理解本发明的内容,但这些具体实施方式不以任何方式限制本发明的保护范围。
实施例1 一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法,包括如下步骤:
(1)将0.004 mol五氯化铌溶于25 mL无水乙醇中,搅拌得到澄清溶液;
(2)称量0.006 mol硝酸镉溶于25 mL去离子水中,搅拌得到澄清溶液;
(3)将以上两溶液混合搅拌,称取适量1.5 g NaOH溶于25 mL去离子水中后,边超声边逐滴加至混合液中,搅拌10分钟后装入水热釜中,在200℃下水热处理48小时,经洗涤干燥后即可得到Cd2Nb2O7/Cd(OH)2光催化材料。
图1是实例1所得Cd2Nb2O7/Cd(OH)2光催化材料的X射线衍射图谱,表明得到了样品物相为Cd2Nb2O7和Cd(OH)2。图2是实例1所得样品的扫描电子显微镜照片,可以看出样品具有多面体形貌。图3是所得样品在紫外光下对罗丹明的光催化效果图,可以看出在120 min后Cd2Nb2O7/Cd(OH)2即可降解掉~80%的RhB,说明所得Cd2Nb2O7/Cd(OH)2具有优异的光催化性能。
实施例2
一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法,包括如下步骤:
(1)将0.0025 mol五氯化铌溶于25 mL无水乙醇中,搅拌得到澄清溶液;
(2)称量0.00625 mol硝酸镉溶于25 mL去离子水中,搅拌得到澄清溶液;
(3)将以上两溶液混合搅拌,称取适量1.2 g NaOH溶于25 mL去离子水中后,边超声边逐滴加至混合液中,搅拌10分钟后装入水热釜中,在180℃下水热处理60小时,经洗涤干燥后即可得到Cd2Nb2O7/Cd(OH)2光催化材料。
实施例3
一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法,包括如下步骤:
(1)将0.005 mol五氯化铌溶于25 mL无水乙醇中,搅拌得到澄清溶液;
(2)称量0.0075 mol硝酸镉溶于25 mL去离子水中,搅拌得到澄清溶液;
(3)将以上两溶液混合搅拌,称取适量1.8 g NaOH溶于25 mL去离子水中后,边超声边逐滴加至混合液中,搅拌10分钟后装入水热釜中,在240℃下水热处理36小时,经洗涤干燥后即可得到Cd2Nb2O7/Cd(OH)2光催化材料。
当然,本发明的上述实施例仅为说明本发明所作的举例,而并非是对本发明的具体实施方式的限定。对于所属领域的普通技术人员来说,在上述举例的基础上还可以做其他不同形式的变化或变动。这里无法对所有的实施方式予以详细举例。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
该专利的研发受到山东省高等学校科技计划(J15LA10)和聊城大学大学生科技创新基金(26312171911)的资助。
Claims (4)
1.一种Cd2Nb2O7/Cd(OH)2光催化材料的制备方法,其特征在于,步骤如下:
(1)将适量的五氯化铌溶于25 mL无水乙醇中,搅拌得到澄清溶液,五氯化铌的摩尔浓度为0.1-0.2 mol/L;
(2)称量适量硝酸镉溶于25 mL去离子水中,搅拌得到澄清溶液,其中溶液中硝酸镉的摩尔浓度为五氯化铌的1.5-2.5倍;
(3)将以上两溶液混合搅拌,称取适量1.2-1.8 g NaOH溶于25 mL去离子水中后,加至混合液中,搅拌10分钟后装入水热釜中,在180-240℃下水热处理36-60小时,经洗涤干燥后即可得到Cd2Nb2O7/Cd(OH)2光催化材料。
2.如权利要求1所述的制备方法,其特征在于,步骤(1)所得五氯化铌的摩尔浓度为0.16mol/L。
3.如权利要求1所述的制备方法,其特征在于,步骤(2)所得溶液中硝酸镉的摩尔浓度为五氯化铌的1.5倍。
4.如权利要求1所述的制备方法,其特征在于,步骤(3)在200℃下水热处理48小时。
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