CN113816432B - 一种纳米片自组装球状钼酸亚铁材料及其制备方法和应用 - Google Patents
一种纳米片自组装球状钼酸亚铁材料及其制备方法和应用 Download PDFInfo
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- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 54
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 41
- 239000002135 nanosheet Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 14
- 239000011733 molybdenum Substances 0.000 claims abstract description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- 239000002638 heterogeneous catalyst Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- OWEGWHBOCFMBLP-UHFFFAOYSA-N 1-(4-chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethylbutan-2-one Chemical compound C1=CN=CN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 OWEGWHBOCFMBLP-UHFFFAOYSA-N 0.000 claims description 5
- 229960003344 climbazole Drugs 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002064 nanoplatelet Substances 0.000 claims description 3
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 230000004913 activation Effects 0.000 claims 1
- 239000000356 contaminant Substances 0.000 claims 1
- XBDUTCVQJHJTQZ-UHFFFAOYSA-L iron(2+) sulfate monohydrate Chemical compound O.[Fe+2].[O-]S([O-])(=O)=O XBDUTCVQJHJTQZ-UHFFFAOYSA-L 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
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- 239000000047 product Substances 0.000 description 6
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- WQKHTJFZNMYFQC-UHFFFAOYSA-L dichloroiron;hydrate Chemical compound O.Cl[Fe]Cl WQKHTJFZNMYFQC-UHFFFAOYSA-L 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000012425 OXONE® Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal molybdate Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明属于无机功能材料的合成技术领域，公开了一种纳米片自组装球状钼酸亚铁(FeMoO4)材料及其制备方法和应用。该方法是将亚铁源、钼源和硫脲按比例溶解于去离子水中，经搅拌和超声充分溶解后，将反应物料转移到微波水热特制反应釜中，于微波反应器中进行水热反应，反应结束后冷却至室温，产物经洗涤、干燥，即可制得纳米片自组装球状钼酸铁。与现有技术相比，本发明提供的技术路线简单、快速，无需调节pH值，反应速率高，产物形貌规整。本发明提供的纳米片自组装球状钼酸亚铁材料作为异相催化剂用于催化降解水中有机污染物，具有优异的催化活性和稳定性，以及制备工艺简单、成本低廉的优点。
Description
技术领域
本发明属于无机功能材料的合成技术领域，特别涉及一种纳米片自组装球状钼酸亚铁(FeMoO4)材料及其制备方法和应用。
背景技术
由于过渡金属钼酸盐具有良好的化学稳定性、环境友好和特殊结构等优点，在催化、磁性、气敏、水处理及能源领域都受到了广泛的关注。钼酸亚铁(FeMoO4)是一类含二价铁的化合物，是一类颇具应用前景的异相催化剂。然而，由于二价铁的不稳定性，且钼酸亚铁为对称性较低的单斜晶系，热力学稳定性较低，合成形貌可控的纯相钼酸亚铁面临巨大的挑战。目前，只有少数研究报道了分级空心球(CrystEngComm,2012,14,7025–7030)、纳米棒(Chemcomm,2020,56,6834-6837)和纳米立方体(Small,2015,36,4753-4761)形貌的钼酸亚铁。
发明内容
为了克服现有钼酸亚铁合成材料技术中存在的缺点和不足，本发明的首要目的在于提供一种纳米片自组装球状钼酸亚铁材料的制备方法。
本发明的另一目的在于提供上述方法制备得到的纳米片自组装球状钼酸亚铁材料。
本发明的再一目的在于提供上述纳米片自组装球状钼酸亚铁材料的应用。该钼酸亚铁材料可以作为活化过硫酸盐(过硫酸钾、过一硫酸氢钾)的异相催化剂用于降解有机污染物具有优异的催化活性。
本发明的目的通过下述技术方案实现：
一种纳米片自组装球状钼酸亚铁材料的制备方法，所包括以下步骤：
(1)将钼源与硫脲(CH4N2S)按摩尔比1：(15～40)充分溶解于去离子水中形成溶液；
(2)以亚铁盐为铁源，将亚铁盐溶于去离子水中，加入步骤(1)所得溶液中，得到反应混合液；
(3)将反应混合液充分搅拌，超声混匀后，转移到微波水热反应釜中，并在微波反应器中进行微波反应；
(4)反应结束后冷却，离心收集冷却后的产物，用无水乙醇和去离子水多次循环清洗，干燥后得到纳米片自组装球状钼酸亚铁材料。
步骤(1)中所述钼源为七钼酸铵((NH4)6Mo7O24)、钼酸钠(Na2MoO4)或钼酸(H2MoO4·H2O)。
步骤(2)中所述亚铁盐为水合硫酸亚铁(FeSO4·7H2O)、水合氯化亚铁(FeCl2·4H2O)、水合硝酸亚铁(Fe(NO3)2·6H2O)或水合乙酸亚铁(Fe(CH3COO)2·4H2O)。
步骤(1)中所述钼源与步骤(2)中所述铁源的摩尔比例为1:(0.8～1.5)。
步骤(1)中所述钼源的摩尔量为0.5～2.0mmol；
步骤(3)中所述搅拌的时间为15～30min；所述超声的时间10～15min；所述微波反应的温度为220～240℃，微波反应的时间为30～60min，微波功率是500～700W。
步骤(4)中所述循环清洗的次数是3次；所述干燥是在烘箱中60℃条件下进行干燥。
一种由上述的制备方法制备得到的纳米片自组装球状钼酸亚铁材料，其特征在于：所述球状钼酸亚铁材料为尺寸1.3～1.8μm的微米颗粒。
上述的纳米片自组装球状钼酸亚铁材料作为活化过硫酸盐(过硫酸钾或过一硫酸氢钾)的异相催化剂在催化降解水中有机污染物中的应用。例如可以将氯咪巴唑快速地(10min以内)完全去除
与现有技术相比，本发明具有以下优点和有益效果：
(1)本发明采用微波水热法简单的方法，高效快速制备了一种纳米片自组装球状钼酸亚铁材料，所提供的技术路线操作简单、快速，无需调节pH值，产物形貌规整、纯度高、催化性能优异，为钼酸亚铁材料的高效简便合成提供了一定的技术支持。
(2)本发明提供的纳米片自组装球状钼酸亚铁材料作为异相催化剂应用于催化降解水中有机污染物(如氯咪巴唑)，具有良好的吸附性能、优异的催化活性和稳定性，以及制备工艺简单、成本低廉的优点。
附图说明
图1为纳米片自组装球状钼酸亚铁的X射线衍射(XRD)图谱。
图2为纳米片自组装球状钼酸亚铁的扫描电子显微镜图(SEM)。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明提供一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，下面结合附图和实施例对本发明进行详细的说明，但本发明的实施方式不限于此。下述实施例中所用的材料、试剂等，如无特殊说明，均可从商业途径得到。
实施例1：
本实施例提供了一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，包括以下步骤：
首先，以七钼酸铵((NH4)6Mo7O24)为钼源，称取1.0mmol的量溶解于20mL去离子水中进行溶解，此时加入硫脲(30mmol)不断搅拌充分混合均匀；同时，将1.0mmol水合硫酸亚铁(FeSO4·7H2O)溶于15mL去离子水中(钼源与铁源的摩尔比为1：1)，并缓慢加入到钼盐与硫脲的混合溶液中；将反应液于室温下充分搅拌20min，超声5min后，将反应前驱体反应液转移到微波水热特制反应釜中，并置于微波反应器中反应，微波反应温度为220℃，反应时间为60min；微波功率是600W；待反应结束后冷却，离心收集冷却后的产物，用去离子水和无水乙醇反复清洗多次，最后于烘箱中60℃干燥得到所述纳米片自组装球状钼酸亚铁，其XRD如图1所示，扫镜电子显微镜图像如图2所示。
使用本实施例制备的钼酸亚铁材料，将其作为异相催化剂应用于催化降解水中有机污染物氯咪巴唑，具有良好的吸附性能，加入过硫酸盐(过硫酸钾或过一硫酸氢钾)后，表现出优越的异相催化性能，2min内可将浓度为2μmol L-1的氯咪巴唑迅速去除，其去除率达100％。
实施例2：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，钼源使用Na2MoO4。
实施例3：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，亚铁盐使用水合氯化亚铁(FeCl2·4H2O)。
实施例4：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，亚铁盐使用水合硝酸亚铁(Fe(NO3)2·6H2O)。
实施例5：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，亚铁盐使用水合乙酸亚铁(Fe(CH3COO)2·4H2O)。
实施例6：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，(NH4)6Mo7O24的摩尔浓度为0.5mmol。
实施例7：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，(NH4)6Mo7O24的摩尔量为2mmol。
实施例8：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，钼源与铁源的摩尔比例1：0.8。
实施例9：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，钼源与铁源的摩尔比例1：1.5。
实施例10：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，微波反应温度为230℃。
实施例11：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，微波反应温度为240℃。
实施例12：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，微波反应时间为30min。
实施例13：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，微波功率为500W。
实施例14：
本实施例一种纳米片自组装球状钼酸亚铁(FeMoO4)材料的制备方法，其制备方法同实施例1的制备方法，不同的是，微波功率为700W。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (8)
1.一种纳米片自组装球状钼酸亚铁材料的制备方法，其特征在于所包括以下步骤：
（1）将钼源与硫脲按摩尔比1：（15~40）充分溶解于去离子水中形成溶液；
（2）以亚铁盐为铁源，将亚铁盐溶于去离子水中，加入步骤（1）所得溶液中，得到反应混合液；
所述钼源与所述铁源的摩尔比例为1:（0.8~1.5）；
（3）将反应混合液充分搅拌，超声混匀后，转移到微波水热反应釜中，并在微波反应器中进行微波反应；所述微波反应的温度为220~240 ℃，微波反应的时间为30~60 min，微波功率是500~700 W；
（4）反应结束后冷却，离心收集冷却后的产物，用无水乙醇和去离子水多次循环清洗，干燥后得到纳米片自组装球状钼酸亚铁材料。
2.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述钼源为七钼酸铵、钼酸钠或钼酸。
3.根据权利要求1所述的制备方法，其特征在于：步骤（2）中所述亚铁盐为水合硫酸亚铁、水合氯化亚铁、水合硝酸亚铁或水合乙酸亚铁。
4.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述钼源的摩尔量为0.5~2.0 mmol。
5.根据权利要求1所述的制备方法，其特征在于：步骤（3）中所述搅拌的时间为15~30min；所述超声的时间10~15 min。
6.根据权利要求1所述的制备方法，其特征在于：步骤（4）中所述循环清洗的次数是3次；所述干燥是在烘箱中60 ℃条件下进行干燥。
7.一种由权利要求1-6任一项所述的制备方法制备得到的纳米片自组装球状钼酸亚铁材料，其特征在于：所述球状钼酸亚铁材料为尺寸1.3~1.8 μm的微米颗粒。
8.根据权利要求7所述的纳米片自组装球状钼酸亚铁材料作为活化过硫酸盐的异相催化剂在催化降解水中有机污染物氯咪巴唑中的应用。
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