CN105664992A - 一种氮掺杂二氧化钛纳米片光催化剂的制备方法 - Google Patents
一种氮掺杂二氧化钛纳米片光催化剂的制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000002135 nanosheet Substances 0.000 title claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 150000003863 ammonium salts Chemical class 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
- 150000002696 manganese Chemical class 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
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- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
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- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
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- 239000002055 nanoplate Substances 0.000 description 9
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- 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 6
- 229940043267 rhodamine b Drugs 0.000 description 6
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
本发明公开了一种无贵金属掺杂、成本低、制备简单、光催化活性高的光催化剂的制备方法。属于新型纳米功能材料与绿色能源技术领域。本发明所制备的氮掺杂二氧化钛纳米片光催化剂为铁和锰双金属原位复合的氮掺杂二氧化钛纳米片FeMn-NTiO2，具有良好的光催化活性。
Description
技术领域
本发明涉及一种氮掺杂二氧化钛纳米片光催化剂的制备方法。属于新型纳米功能材料与绿色能源技术领域。
背景技术
光催化剂，也被称为光触媒，是一种在光的照射下，自身不起变化，却可以促进化学反应的物质。光触媒是利用自然界存在的光能转换成为化学反应所需的能量，来产生催化作用，使周围之氧气及水分子激发成极具氧化力的自由负离子。几乎可分解所有对人体和环境有害的有机物质及部分无机物质，不仅能加速反应，亦能运用自然界的定侓，不造成资源浪费与附加污染形成。世界上能作为光触媒的材料众多，包括二氧化钛、氧化锌、氧化锡、二氧化锆、硫化镉等多种氧化物硫化物半导体，其中二氧化钛（TiO2）因其氧化能力强，化学性质稳定无毒，成为世界上最当红的纳米光触媒材料。
然而，要充分发挥二氧化钛的实际应用水平，需要一方面通过调控其材料形貌以暴露更多高活性晶面来提高光催化活性，另一方面通过掺杂不同金属或金属氧化物调控光敏波长向可见光范围扩展来提高太阳光的利用率。因此，研发成本低、制备简单的高光催化活性的二氧化钛光触媒具有重要的科学意义和应用价值。
根据目前的研究，由于片状二氧化钛纳米材料能够暴露更多的高指数晶面，具有更高的光催化活性，二氧化钛纳米片具有比纳米粒子更好地应用前景，对于二氧化钛纳米片的研究也备受关注。而单一的二氧化钛纳米材料的光敏波长一般在紫外区，而且由于不容易分散而容易互相影响而降低光催化活性，不利于实际应用。但是，在二氧化钛纳米材料上修饰或复合特殊的纳米材料，可以有效提高光生载流子对的有效浓度，提高光电转换效率，提高光催化活性。因此，设计、制备高效、稳定的二氧化钛纳米片及其修饰物是制备二氧化钛光触媒的关键技术。
发明内容
本发明的目的在于提供一种无贵金属掺杂、成本低、制备简单、光催化活性高的光催化剂。
本发明采用的技术方案如下：
一种氮掺杂二氧化钛纳米片光催化剂的制备方法，所述的氮掺杂二氧化钛纳米片光催化剂为铁和锰双金属原位复合的氮掺杂二氧化钛纳米片FeMn-NTiO2，其特征在于，所述的FeMn-NTiO2的制备步骤为：
首先，取0.8mmol铁盐、0.8~1.2mmol锰盐和1mmol铵盐加入到5mL钛酸四丁酯中，搅拌过程中，缓慢加入0.5~0.8mL氢氟酸，160~200℃下在反应釜中反应18~24小时，冷却至室温后，用超纯水和无水乙醇离心洗涤三次后，50℃下真空干燥；然后，将研磨的粉末放入马弗炉中，升温速度为1~3℃/min，480~560℃下在氮气保护下，煅烧10~60min；最后，将煅烧后的粉末冷却至室温，即制得FeMn-NTiO2；
所述的铁盐选自下列之一：硫酸铁、氯化铁、硝酸铁；
所述的锰盐选自下列之一：硫酸锰、氯化锰、硝酸锰；
所述的铵盐选自下列之一：硫酸铵、氯化铵、硝酸铵、碳酸铵。
本发明的有益成果
（1）本发明所述的光催化剂制备方法简单、快速，无贵金属掺杂、成本低，具有市场发展前景；
（2）本发明首次制备了新型光敏材料FeMn-NTiO2，由于铁、锰在二氧化钛纳米片上的原位生长而充分与二氧化钛纳米片接触，利用铁、锰的金属表面等离子体作用以及二者的相互促进作用，有效阻止了光生电子-空穴对的复合，极大地提高了光催化活性，由于金属离子的作用，拓宽了光敏波长地范围，提高了太阳光地利用效率，解决了二氧化钛纳米片虽然光催化效果好，但是在太阳光照射下光催化效果差的技术问题；同时由于氮的掺杂而使得二氧化钛纳米片更好的加大层隙间距和充分分散，极大地增大了二氧化钛纳米片的光催化活性和解决了二氧化钛纳米片不利于分散而降低光催化活性的技术问题，因此，该材料的有效制备，具有重要的科学意义和应用价值；
（3）本发明制备的光催化剂FeMn-NTiO2，该材料除了具有高效的光电转化效率，而且自身的生物相容性好、大的比表面积、高的表面介孔吸附特性，可以作为基质材料，制备各类传感器，如光电化学传感器、电致化学发光传感器、电化学传感器等，具有广泛的潜在使用价值。
具体实施方式
实施例1FeMn-NTiO2的制备
首先，取0.8mmol铁盐和0.8mmol锰盐和1mmol铵盐加入到5mL钛酸四丁酯中，搅拌过程中，缓慢加入0.5mL氢氟酸，160℃下在反应釜中反应24小时，冷却至室温后，用超纯水和无水乙醇离心洗涤三次后，50℃下真空干燥；然后，将研磨的粉末放入马弗炉中，升温速度为1℃/min，在480℃下煅烧60min；最后，将煅烧后的粉末冷却至室温，即制得FeMn-NTiO2；
所述的铁盐为硫酸铁；
所述的锰盐为硫酸锰；
所述的铵盐为硫酸铵。
实施例2FeMn-NTiO2的制备
首先，取0.8mmol铁盐和1.0mmol锰盐和1mmol铵盐加入到5mL钛酸四丁酯中，搅拌过程中，缓慢加入0.65mL氢氟酸，180℃下在反应釜中反应21小时，冷却至室温后，用超纯水和无水乙醇离心洗涤三次后，50℃下真空干燥；然后，将研磨的粉末放入马弗炉中，升温速度为2℃/min，在520℃下煅烧30min；最后，将煅烧后的粉末冷却至室温，即制得FeMn-NTiO2；
所述的铁盐为氯化铁；
所述的锰盐为氯化锰；
所述的铵盐为氯化铵。
实施例3FeMn-NTiO2的制备
首先，取0.8mmol铁盐和1.2mmol锰盐和1mmol铵盐加入到5mL钛酸四丁酯中，搅拌过程中，缓慢加入0.8mL氢氟酸，200℃下在反应釜中反应18小时，冷却至室温后，用超纯水和无水乙醇离心洗涤三次后，50℃下真空干燥；然后，将研磨的粉末放入马弗炉中，升温速度为3℃/min，在560℃下煅烧10min；最后，将煅烧后的粉末冷却至室温，即制得FeMn-NTiO2；
所述的铁盐为硝酸铁；
所述的锰盐为硝酸锰；
所述的铵盐为硝酸铵。
实施例4FeMn-NTiO2的光催化活性测试
以500W卤钨灯为光源，距离光催化反应器约10cm，光源与反应器之间置一滤光片，截掉波长小于420nm的光。将0.05g实施例1制备的FeMn-NTiO2加入到50mL浓度为0.01mmol/L的罗丹明B溶液中，超声分散10min，然后将料液置于暗室中搅拌0.5小时，确保样品表面吸附达到吸附-脱附平衡后，在光照下搅拌进行反应。每隔30min取样，用孔径0.45μm的滤膜过滤，用紫外-可见分光光度计测定滤液在波长为554nm处的吸光度，根据溶液浓度与吸光度成正比计算不同反应时间的罗丹明B溶液浓度和降解率，实验130min后脱色率达到99.6%，说明本发明所制备的FeMn-NTiO2具有实际应用价值。
实施例5FeMn-NTiO2的光催化活性测试
以500W卤钨灯为光源，距离光催化反应器约10cm，光源与反应器之间置一滤光片，截掉波长小于420nm的光。将0.05g实施例2制备的FeMn-NTiO2加入到50mL浓度为0.01mmol/L的罗丹明B溶液中，超声分散10min，然后将料液置于暗室中搅拌0.5小时，确保样品表面吸附达到吸附-脱附平衡后，在光照下搅拌进行反应。每隔30min取样，用孔径0.45μm的滤膜过滤，用紫外-可见分光光度计测定滤液在波长为554nm处的吸光度，根据溶液浓度与吸光度成正比计算不同反应时间的罗丹明B溶液浓度和降解率，实验130min后脱色率达到99.6%，说明本发明所制备的FeMn-NTiO2具有实际应用价值。
实施例6FeMn-NTiO2的光催化活性测试
以500W卤钨灯为光源，距离光催化反应器约10cm，光源与反应器之间置一滤光片，截掉波长小于420nm的光。将0.05g实施例3制备的FeMn-NTiO2加入到50mL浓度为0.01mmol/L的罗丹明B溶液中，超声分散10min，然后将料液置于暗室中搅拌0.5小时，确保样品表面吸附达到吸附-脱附平衡后，在光照下搅拌进行反应。每隔30min取样，用孔径0.45μm的滤膜过滤，用紫外-可见分光光度计测定滤液在波长为554nm处的吸光度，根据溶液浓度与吸光度成正比计算不同反应时间的罗丹明B溶液浓度和降解率，实验130min后脱色率达到99.6%，说明本发明所制备的FeMn-NTiO2具有实际应用价值。
Claims (1)
1.一种氮掺杂二氧化钛纳米片光催化剂的制备方法，所述的氮掺杂二氧化钛纳米片光催化剂为铁和锰双金属原位复合的氮掺杂二氧化钛纳米片FeMn-NTiO2，其特征在于，所述的FeMn-NTiO2的制备步骤为：
首先，取0.8mmol铁盐、0.8~1.2mmol锰盐和1mmol铵盐加入到5mL钛酸四丁酯中，搅拌过程中，缓慢加入0.5~0.8mL氢氟酸，160~200℃下在反应釜中反应18~24小时，冷却至室温后，用超纯水和无水乙醇离心洗涤三次后，50℃下真空干燥；然后，将研磨的粉末放入马弗炉中，升温速度为1~3℃/min，480~560℃下在氮气保护下，煅烧10~60min；最后，将煅烧后的粉末冷却至室温，即制得FeMn-NTiO2；
所述的铁盐选自下列之一：硫酸铁、氯化铁、硝酸铁；
所述的锰盐选自下列之一：硫酸锰、氯化锰、硝酸锰；
所述的铵盐选自下列之一：硫酸铵、氯化铵、硝酸铵、碳酸铵。
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