CN107827153B - 一种纳米钒酸银的制备方法 - Google Patents
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- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 16
- 229910003206 NH4VO3 Inorganic materials 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000002738 chelating agent Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 239000013522 chelant Substances 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- -1 silver vanadates Chemical class 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
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- B01J35/39—
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
本发明属于催化材料制备领域，具体涉及一种纳米钒酸银的制备方法。本发明所要解决的技术问题是提供一种纳米钒酸银的制备方法，包括以下步骤：在NH4VO3水溶液中加入螯合剂、表面活性剂溶解完全后，再加入硝酸银水溶液，搅拌混匀得到前驱体溶液；前驱体溶液在室温或加热条件下反应后，沉淀，过滤得固体，即为纳米钒酸银。本发明方法操作简单，能够制得纳米级的钒酸银。
Description
技术领域
本发明属于催化材料制备领域，具体涉及一种纳米钒酸银的制备方法。
背景技术
近年来，环境污染问题尤其是水污染问题日趋严重，已经对人类的生存和发展造成了严重的威胁。因此有效治理环境污染，使人类的生存环境得到改善，已经成为全球关注的焦点。近年来，在半导体光催化剂的研究中，钒酸银以其优异的可见光光催化性能，引起了国内外学者们的关注。目前，钒酸银的制备方法主要有：水热法、固相反应法和共沉淀法等。
公开号为“CN102941090B”的中国专利中公开了一种双注沉淀法制备棒状钒酸银光催化材料的制备方法，即在高分子保护剂存在下，将硝酸银和氨水的混合溶液与钒酸钠溶液同时注入含有钒酸银的反应锅中反应，但技术难度大，且对所制备的产品保存条件要求高。公开号为“CN 106191903 A”的中国专利公开了一种沉淀辅助微波水热法快速合成Ag3VO4纳米光催化剂的方法，化学组成均一，纯度较高，具有较大的比表面积，但不适合于大规模生产制备；中国发明201310257173.7公开了一种钒酸银纳米纤维光催化剂及其制备方法，采用静电纺丝法制备，但对水分等要求高，技术难度大。CTAB-assisted hydrothermalsynthesis of silver vanadates and their photocatalyticcharacterization.Chao-Ming Huang等人采用CTAB作为表面活性剂的水热结合热处理方式制备得到Ag3VO4与Ag4V2O7的混合相，其产品纯度不高，且尺寸较大。
钒酸银作为新型的可见光响应的光催化剂，因其良好的可见光光催化活性而受到科研工作者的广泛关注。以上方法均存在操作复杂、添加剂繁多、材料制备周期长、不易分离的问题，不适合于大规模生产，目前用于制备钒酸银的方法还很有限，因此采用新的方法，制备出具有不同形貌、能在可见光下高效率地降解有机污染物的钒酸银光催化剂具有很重要的实际意义。
发明内容
针对现有方法制备钒酸银存在的问题，本发明提供了一种钒酸银纳米颗粒的制备方法。
本发明所要解决的技术问题是提供一种纳米钒酸银的制备方法。该方法包括以下步骤：在NH4VO3水溶液中加入螯合剂、表面活性剂，溶解完全后加入硝酸银水溶液，搅拌，得到前驱体溶液；前驱体溶液在室温或加热条件下反应，析出沉淀，过滤得固体，即为纳米钒酸银。
优选的，上述纳米钒酸银的制备方法中，所述的加热采用微波的方式。
进一步的，上述纳米钒酸银的制备方法中，所述微波的功率为600～1200W，频率2450MHz，时间为5～30min。
优选的，上述纳米钒酸银的制备方法中，所述搅拌的时间为2～6h。
优选的，上述纳米钒酸银的制备方法中，所述NH4VO3水溶液浓度为0.1～0.5mol/L。
优选的，上述纳米钒酸银的制备方法中，所述硝酸银水溶液浓度为0.1～0.5mol/L。
优选的，上述纳米钒酸银的制备方法中，所述表面活性剂的加入量为NH4VO3质量的0.5～2％。
优选的，上述纳米钒酸银的制备方法中，所述表面活性剂为CTAB或聚丙烯酸至少一种。
优选的，上述纳米钒酸银的制备方法中，所述螯合剂的加入量为NH4VO3质量的5～10％。
优选的，上述纳米钒酸银的制备方法中，所述螯合物为草酸、苹果酸、柠檬酸、丙三醇、EDTA或NTA中的至少一种。
优选的，上述纳米钒酸银的制备方法中，所述NH4VO3与硝酸银的摩尔比为0.9～1.1﹕0.9～1.1。
本发明制备纳米钒酸银的方法，采用NH4VO3和硝酸银为原料，辅以螯合剂和表面活性剂，能够使原料分散均匀，从而得到粒度分布均匀的纳米钒酸银。再配合采用微波处理方式，不仅时间短、易操作，更进一步使产品粒度分布均匀；微波辅助合成，具有简便、快速、高效、绿色等优点。本发明方法能够得到粒度在50～200nm的钒酸银产品，为纳米钒酸银的制备提供了一条更好的选择。
附图说明
图1本发明所得产品XRD图
具体实施方式
本发明方法合成机理为：钒源、螯合剂与银源形成配合物前驱体，加入表面活性剂使成核生长过程局限在一个微小的范围内，粒子的大小、形状、结构等都受到微反应器的组成与结构的影响，为实现纳米粒子的人为调控提供了有利的手段。通过微波加热使前驱体迅速分解制备纳米钒酸银，由于反应速率快，团聚小、粒度分布均匀。
纳米钒酸银的制备方法，包括以下步骤：在NH4VO3水溶液中加入螯合剂、表面活性剂溶解完全后，再加入硝酸银水溶液，混匀，搅拌一段时间后得到前驱体溶液；该前驱体溶液在室温环境下继续搅拌或者采用加热的方式对其进行处理，体系中会产生析出钒酸银沉淀，过滤沉淀，即得纳米钒酸银。
本发明方法中，对前驱体溶液制备得到钒酸银沉淀的条件并无特别限制，在室温下搅拌即可，但是所需时间长，效率低于加热方式。对加热方式也没有特别限定，常规加热方式均可。但为了保证加热的均匀性，优选采用微波加热的方式。
实施例1
称取5gNH4VO3、加入0.25g EDTA、0.05gCTAB在200～400r/min下剧烈搅拌使其溶解，配置成0.2mol/L的NH4VO3水溶液，加入浓度0.2mol/L硝酸银溶液，控制n(V)/n(Ag)＝1﹕1，再搅拌2h，制备前驱体溶液；通过微波辅助合成，反应时间10min，制备出纳米钒酸银。
实施例2
称取2g NH4VO3、加入0.2g草酸、0.04g聚丙烯酸，在300r/min的搅拌速率下使其溶解，配置成0.3mol/L NH4VO3溶液，加入0.1mol/L硝酸银溶液，控制V/Ag＝1.1﹕1(摩尔比)，再搅拌2h，制备前驱体溶液；通过微波辅助合成，反应时间10min，制备出纳米钒酸银。
Claims (5)
1.纳米钒酸银的制备方法，其特征在于：包括以下步骤：在NH4VO3水溶液中加入螯合剂、表面活性剂，溶解完全后加入硝酸银水溶液，搅拌，得到前驱体溶液；前驱体溶液在室温或加热条件下反应，析出沉淀，过滤得固体，即为纳米钒酸银；所述NH4VO3水溶液浓度为0.1～0.5mol/L；所述硝酸银水溶液浓度为0.1～0.5mol/L；所述NH4VO3与硝酸银的摩尔比为0.9～1.1﹕0.9～1.1；所述表面活性剂的加入量为NH4VO3质量的0.5～2％；所述螯合剂的加入量为NH4VO3质量的5～10％；所述螯合物为草酸、苹果酸、柠檬酸、丙三醇、EDTA或NTA中的至少一种。
2.根据权利要求1所述的纳米钒酸银的制备方法，其特征在于：所述的加热采用微波的方式。
3.根据权利要求2所述的纳米钒酸银的制备方法，其特征在于：所述微波的功率为600～1200W，频率2450MHz，时间为5～30min。
4.根据权利要求1所述的纳米钒酸银的制备方法，其特征在于：所述搅拌的时间为2～6h。
5.根据权利要求1～4任一项所述的纳米钒酸银的制备方法，其特征在于：所述表面活性剂为CTAB或聚丙烯酸至少一种。
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