CN107961782B - 一种带有方孔的立方体NaNbO3光催化材料的制备方法 - Google Patents
一种带有方孔的立方体NaNbO3光催化材料的制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 15
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims abstract description 21
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 18
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 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
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
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- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
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- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
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- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 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 2
- 238000003911 water pollution Methods 0.000 description 2
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- MUPJWXCPTRQOKY-UHFFFAOYSA-N sodium;niobium(5+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[Na+].[Nb+5] MUPJWXCPTRQOKY-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种带有方孔的立方体NaNbO3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、氢氧化钠、硝酸钠为原料,在180‑240℃下水热处理36‑60小时,即可制备出带有方孔的立方体NaNbO3光催化材料。具有方孔的立方体形貌有利于对光的吸收和对污染物的吸附,大幅提高了光催化材料的吸附能力,进而提高了光催化降解的速率。本发明所描述的制备方法成本低廉,工艺简单,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,尤其是涉及一种带有方孔的立方体NaNbO3光催化材料的制备。
背景技术
随着全球工农业的快速发展,环境污染和能源问题,特别是水污染中有机污染物亟待处理。如何更为绿色高效地处理被有机污染的水体备受关注。与吸附和过滤等方法相比,基于半导体材料的光催化技术被认为是解决水污染问题最为有效、最有前途的方法之一。光催化技术则是通过吸收太阳光,驱动氧化还原反应,破坏水体中的有害的有机污染物,不会产生二次污染。
NaNbO3是一种铁电性很强的钙钛矿型铁电体,它具有高的电光系数和非线性光学系数,能对近红外半导体激光进行倍频获得蓝光输出,主要用于激光倍频、电光调制和光折变材料,是人们非常感兴趣的一种非线性光学材料。同时,NaNbO3也是禁带宽度为~3.48 eV的半导体材料。最近研究发现,在紫外光激发下,展现出比TiO2更高的光催化降解能力。为了更好地利用紫外光,研究工作者进行了大量的探索,通过金属修饰、构建异质结等手段,以提高其紫外光催化性能。
本发明制备了带有方孔的立方体NaNbO3光催化材料。该催化材料制备方法仅是通过以五氯化铌、氢氧化钠、硝酸钠为原料,在180-240℃下水热处理36-60小时,即可得到带有方孔的立方体NaNbO3。开孔形貌不仅使材料具有更高的比表面积,另外还可以更有效地捕获紫外激发光,进而极大地提高光催化活性;另外,该方法还具有成本低、过程简单和易于操作的特点。
发明内容
本发明制备出了一种带有方孔的立方体NaNbO3光催化材料,所得光催化材料具有高的紫外光催化活性,在污水处理等领域有着潜在应用;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。
本发明涉及一种带有方孔的立方体NaNbO3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0.1-0.3 mol/L;
(2)称量适量硝酸钠溶于25 mL去离子水中,搅拌得到澄清溶液,溶液中硝酸钠的摩尔浓度为五氯化铌的3-5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带有方孔的立方体NaNbO3光催化材料。
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)所得溶液中硝酸钠的摩尔浓度为五氯化铌的4倍。
优选的,步骤(3)在200℃下水热处理48小时。
该制备方法温度低,过程简单,易于操作,可连续化生产;该方法制得的NaNbO3光催化材料具有带有方孔的立方体形貌和优异的紫外光催化性能。
本发明取得的优异效果是:
1. 该方法制得的带有方孔的立方体NaNbO3光催化材料,具有高的紫外光催化活性,在环境保护领域有着潜在应用前景;
2. 本发明描述的制备方法成本低,过程简单,易于操作,不需要复杂设备。
附图说明
图1是实施例1制备的带有方孔的立方体NaNbO3光催化材料的X射线衍射图谱;
图2是实施例1制备的带有方孔的立方体NaNbO3光催化材料对罗丹明B的降解效果图;
图3是实施例1制备的带有方孔的立方体NaNbO3的扫描电子显微镜照片。
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 一种带有方孔的立方体NaNbO3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,五氯化铌的摩尔浓度为0.16 mol/L。
(2)称量0.012 mol硝酸钠溶于25 mL去离子水中,搅拌得到澄清溶液,溶液中硝酸钠的摩尔浓度为五氯化铌的3倍;
(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,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带有方孔的立方体NaNbO3光催化材料。
图1是实例1所得NaNbO3的X射线衍射图谱,表明得到了样品物相为NaNbO3。图2是实例1所得NaNbO3对罗丹明的紫外光催化效果图,可以看出在100 min光照下NaNbO3对RhB降解率达到100%,说明所得NaNbO3具有优异的光催化性能。图3为实例1所得NaNbO3的扫描电子显微镜照片,可以看出NaNbO3光催化材料的带有方孔的立方体形貌。
实施例2
一种带有方孔的立方体NaNbO3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,五氯化铌的摩尔浓度为0.1 mol/L。
(2)称量0.0125 mol硝酸钠溶于25 mL去离子水中,搅拌得到澄清溶液,溶液中硝酸钠的摩尔浓度为五氯化铌的5倍;
(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,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带有方孔的立方体NaNbO3光催化材料。
实施例3
一种带有方孔的立方体NaNbO3光催化材料的制备方法,包括如下步骤:
(1)将0.0075 mol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0.3 mol/L。
(2)称量0.03 mol硝酸钠溶于25 mL去离子水中,搅拌得到澄清溶液,溶液中硝酸钠的摩尔浓度为五氯化铌的4倍;
(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,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带有方孔的立方体NaNbO3光催化材料。
以上各实施例只是对本发明做进一步说明,并非用以限制本发明专利,凡为本发明的等效实施,均应包含于本发明专利的权利要求范围之内。
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)
1.一种带有方孔的立方体NaNbO3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0.1-0.3 mol/L;
(2)称量适量硝酸钠溶于25 mL去离子水中,搅拌得到澄清溶液,溶液中硝酸钠的摩尔浓度为五氯化铌的3-5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带有方孔的立方体NaNbO3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)所得溶液中硝酸钠的摩尔浓度为五氯化铌的4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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Synthesis and enhanced photocatalytic activity of NaNbO3 prepared by hydrothermal and polymerized complex methods;Li Guoqiang,et al.;《Journal of Physics and Chemistry of Solids》;20081031;第69卷;全文 * |
铌酸钠和铌酸镉的水热合成与表征;李雪璨;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20141015;第2.2.2节和图2.2 * |
铌酸钠粉体的水热法制备及其光催化性能研究;金姣;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20130615;第2.2.2,2.3.3和2.3.4节 * |
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