CN107159185A - 一种用于降解罗丹明b的三氧化钼催化剂及其制备方法 - Google Patents
一种用于降解罗丹明b的三氧化钼催化剂及其制备方法 Download PDFInfo
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 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 title claims abstract description 24
- 229940043267 rhodamine b Drugs 0.000 title claims abstract description 23
- 230000015556 catabolic process Effects 0.000 title claims abstract description 18
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002086 nanomaterial Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- -1 Ammonium Molybdate Tetrahydrates Chemical class 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 3
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
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- 235000009566 rice Nutrition 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 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 description 3
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910003149 α-MoO3 Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
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- B01J23/28—Molybdenum
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Abstract
本发明涉及一种用于降解罗丹明B的三氧化钼催化剂及其制备方法，属于纳米材料制备技术领域。本发明包括两个步骤：(1)采用水热法一步制备得到三氧化钼(MoO3)纳米材料；(2)所制备的三氧化钼具有由纳米片组装成的三维多级纳米花结构，对罗丹明B表现出高效优异的降解性能。50毫克三氧化钼催化剂对100毫升，20毫克每升罗丹明B溶液，在可见光条件下，160分钟光催化降解可达到91.53％的降解率。本发明的方法操作简单易行，可大量生产，具有广阔的应用前景。
Description
技术领域
本发明涉及纳米材料制备技术领域，具体说涉及一种用于降解罗丹明B的三氧化钼催化剂及其制备方法。
背景技术
随着生活质量的提高，人类自身的安全与环境问题越来越受到重视，水体中的有机污染物即是其中的热点被关注对象之一。金属氧化物半导体因其在光催化方面高效、简单与低能耗等特点，在降解水体中的有机污染领域得到广泛应用。在金属氧化物半导体对水体中的有机污染成分进行光催化降解时，只需要可见光的照射即可；常用于光催化的金属氧化物半导体有二氧化钛(TiO2)、三氧化钨(WO3)、氧化铋(Bi2O3)等。但材料自身的特性对于光催化降解的所需的条件仍有不同，如TiO2因为稳定、无毒、高效的特点而被广泛使用于光催化方面，但TiO2只能吸收紫外光，而太阳光中仅有4％的紫外光，因此，开发能吸收可见光降解有机染料的催化剂是很有必要的。
三氧化钼(MoO3)是一种宽禁带宽度的N型半导体，被广泛应用于电致变色、热致变色、光致变色、气敏传感器、催化剂等方面；另外，MoO3也是合成MoO2，MoS2，MoSe2和Mo等重要材料的良好前驱体。MoO3常见的相有三种：稳定态的正交相三氧化钼(α-MoO3)，亚稳定态的单斜相三氧化钼(β-MoO3)与六方相三氧化钼(h-MoO3)[T.Itoh,I.Matsubara,W.Shin,N.Izuand M.Nishibori,Sens.Actuators,B,2008,128,512-520；D.Mariotti,H.A.C.Bose, and K.K.Ostrikov,Nanotechnology,2008,19,495302-495307；L.Zheng,Y.Xu,D.Jin and Y.Xie, Chem.Mater.,2009,21,5681-5690]。Chen等通过水热合成出α-MoO3纳米带，并用于亚甲基蓝 (MB)的降解实验[Y.P.Chen,C.L.Lu,L.Xu,Y.Ma,W.H.Hou andJ.J.Zhu,CrystEngComm, 2010,12,3740-3747]，Chithambararaj等合成出h-MoO3，用于亚甲基蓝的降解实验，同时 Chithambararaj等也合成出α-MoO3用于亚甲基蓝的降解，并将α-MoO3与h-MoO3的降解情况进行对比，发现在相同条件下h-MoO3的降解情况比α-MoO3更好[A.Chithambararaj,N.S.Sanjini, A.C.Bose and S.Velmathi,Catal.Sci.Technol.,2013,3,1405-1414；A.Chithambararaj,N.S. Sanjini,S.Velmathi and A.C.Bose,Phys.Chem.Chem.Phys.,2013,15,14761-14769]。
本发明所制备出的三氧化钼为三维多级纳米结构，明显具有以下优势：其一，制备三氧化钼的原料易得、方法简单、低能耗；其二，制备的三氧化钼具有三维多级纳米花结构，在降解罗丹明B时，有利于罗丹明B分子与三氧化钼催化剂的接触，进而表现出高效地光催化降解性能。
发明内容
合成一种三维多级结构三氧化钼纳米材料，本发明是这样实现的，采用水热法合成出用于室温下降解有机染料罗丹明B的三氧化钼纳米材料，该材料具有由纳米片组装成的三维多级纳米花结构。
一种用于室温下降解有机染料罗丹明B的三氧化钼的制备方法，其特征在于，采用水热法合成，以四水合钼酸铵为原料，聚乙二醇2000为模板剂，浓盐酸提供酸性环境，制备出三氧化钼纳米材料，其步骤为：
(1)三氧化钼的制备
称取1.2358克四水合钼酸铵与0.4克，聚乙二醇2000加入到100毫升烧杯中，加入30.0 毫升去离子水，加入5.0毫升浓盐酸，在磁力搅拌器上搅拌30分钟，将得到的透明溶液装入 50毫升反应釜中，160摄氏度水热24小时，待冷却至室温，将得到的沉淀产物离心洗涤后置于60摄氏度的烘箱内烘干12小时得到蓝黑色的三氧化钼纳米材料。
(2)光催化降解性质测试
样品的光催化性质是在可见光下降解罗丹明B来评估的，使用的光源为300瓦氙灯，采用λ>420纳米滤光片滤掉紫外光。称取50毫克样品，量取100毫升20毫克每升罗丹明B溶液置于200毫升烧杯内，在黑暗条件下搅拌处理1小时，确定达到吸附/脱附平衡。之后将搅拌状态下的混合液置于氙灯下，在20分钟的时间间隔下，从烧杯中取样5毫升离心分离，取上清液，使用N4紫外可见分光光度计进行吸光光谱测试，利用罗丹明B溶液的吸光度值来表征其浓度随催化时间的变化。根据吸光度值与溶液浓度成正比例的关系，可以得到罗丹明B 的降解率η＝[(c0-ct)/c0]×100％＝[(A0-At)/A0]×100％，其中t时刻罗丹明B溶液的浓度与吸光度值用ct，At表示；罗丹明B溶液的初始浓度与吸光度值用c0，A0表示。
与现有研究成果相比，本发明的优势在于：
1、本发明制备的三氧化钼纳米材料在相同条件下能降解高浓度罗丹明B；
2、本发明制备的三氧化钼纳米材料能高效地降解罗丹明B，160分钟光催化降解可达到91.53％的降解率；
3、本发明制备的三氧化钼纳米材料流程简单、低能耗、无需昂贵设备，原料易得，总体成本低廉。
附图说明
图1是MoO3纳米材料的2700倍扫描电子显微镜图片；
图2是MoO3纳米材料的5500倍扫描电子显微镜图片；
图3是MoO3纳米材料的14000倍扫描电子显微镜图片；
图4是MoO3纳米材料的35000倍扫描电子显微镜图片；
图5是MoO3纳米材料的XRD谱图；
图6是MoO3纳米材料降解的100毫升20毫克每升罗丹明B溶液的吸收曲线。
具体实施方式
本发明所选用四水合钼酸铵，聚乙二醇2000，浓盐酸均为市售分析纯产品，去离子水为实验室自制；所用的玻璃仪器和设备是实验室中常用的仪器和设备。
实施例：称取1.2358克四水合钼酸铵与0.4克，聚乙二醇2000加入到100毫升烧杯中，加入30.0毫升去离子水，加入5毫升浓盐酸，在磁力搅拌器上搅拌30分钟，将得到的透明溶液装入50毫升反应釜中，160摄氏度水热24小时，待冷却至室温，将得到的沉淀产物离心洗涤后置于60摄氏度烘箱内烘干12小时得到蓝黑色粉末即为MoO3，该产物为三维多级纳米花结构，如图1所示；图2-4可以看出该纳米花由纳米片组装而成。
所制备的MoO3纳米材料具有良好的结晶性，其衍射峰的d值和相对强度与MoO3的PDF 标准卡片(76-1003)所列的d值和相对强度一致，属于正交相，如图5所示。
称取50毫克样品，量取100毫升20毫克每升罗丹明B溶液置于200毫升烧杯内，在黑暗条件下搅拌处理1小时，确定达到吸附/脱附平衡，之后在氙灯下照射，在20分钟的时间间隔下，从烧杯中取样5.0毫升进行离心分离，取上清液进行吸光度测试。如图6所示。
当然，本发明还可有其他多种实施例，在不背离本发明精神及其实质的情况下，熟悉本领域的技术人员可根据本发明做出各种相应的改变和变形，但这些相应的改变和变形都应属于本发明所附的权利要求的保护范围。
Claims (3)
1.一种用于降解罗丹明B的三氧化钼催化剂，其特征在于，该材料为三维多级的纳米花结构，将三氧化钼纳米材料进行光催化降解罗丹明B测试，对罗丹明B的降解具有高效性，在催化剂用量为50毫克时，对100毫升20毫克每升罗丹明B溶液，160分钟光催化降解可达到91.53％的降解率。
2.一种如权利要求1所述的三氧化钼纳米材料，其特征在于，该材料具有三维多级的纳米花结构。
3.一种如权利要求1所述的三氧化钼的制备方法，其特征在于，采用水热法，采用水热法合成，以四水合钼酸铵为原料，聚乙二醇2000为模板剂，浓盐酸提供酸性环境，制备出三氧化钼纳米材料。其步骤为：
(1)称取1.2358克四水合钼酸铵与0.4克，聚乙二醇2000加入到100毫升烧杯中；
(2)加入30毫升去离子水，加入5毫升浓盐酸，在磁力搅拌器上搅拌30分钟；
(3)将得到的透明溶液装入50毫升反应釜中，160摄氏度水热24小时；
(4)待冷却至室温，将得到的沉淀产物离心洗涤；
(6)将得到的沉淀置于60摄氏度烘箱内烘干12小时得到蓝黑色的三氧化钼纳米材料；
(7)将三氧化钼纳米材料用于降解罗丹明B的光催化性能测试。
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| CN112978799A (zh) * | 2021-03-24 | 2021-06-18 | 常州工学院 | 一种纯六方相片状三氧化钼纳米吸附剂及其制备方法和应用 |
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| CN111135818A (zh) * | 2019-12-13 | 2020-05-12 | 上海电力大学 | 一种MoO3/ZnAl层状双氢氧化物复合材料的制备方法和产品及其应用 |
| CN111135818B (zh) * | 2019-12-13 | 2022-12-27 | 上海电力大学 | 一种MoO3/ZnAl层状双氢氧化物复合材料的制备方法和产品及其应用 |
| CN112978799A (zh) * | 2021-03-24 | 2021-06-18 | 常州工学院 | 一种纯六方相片状三氧化钼纳米吸附剂及其制备方法和应用 |
| CN113198455A (zh) * | 2021-05-17 | 2021-08-03 | 南昌航空大学 | 一种三氧化钼/钼网光催化剂及其制备方法和应用 |
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