CN114849781B - 一种钴铌氧簇及其制备方法与应用 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XKSCGGSEXVOBRB-UHFFFAOYSA-N [O-2].[Nb+5].[Co+2] Chemical compound [O-2].[Nb+5].[Co+2] XKSCGGSEXVOBRB-UHFFFAOYSA-N 0.000 title abstract description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 27
- 239000011734 sodium Substances 0.000 claims abstract description 14
- 239000002178 crystalline material Substances 0.000 claims abstract description 13
- 239000010955 niobium Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 5
- 239000011780 sodium chloride Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- HLYSAPLLWJJISU-UHFFFAOYSA-K trichlorocobalt hexahydrate Chemical compound O.O.O.O.O.O.Cl[Co](Cl)Cl HLYSAPLLWJJISU-UHFFFAOYSA-K 0.000 claims abstract description 5
- MHUWZNTUIIFHAS-XPWSMXQVSA-N 9-octadecenoic acid 1-[(phosphonoxy)methyl]-1,2-ethanediyl ester Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(COP(O)(O)=O)OC(=O)CCCCCCC\C=C\CCCCCCCC MHUWZNTUIIFHAS-XPWSMXQVSA-N 0.000 claims abstract description 3
- 229940047047 sodium arsenate Drugs 0.000 claims abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 5
- 238000006303 photolysis reaction Methods 0.000 claims description 5
- 230000015843 photosynthesis, light reaction Effects 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002447 crystallographic data Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229940000489 arsenate Drugs 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical class [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
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Abstract
本申请公开一种钴铌氧簇及其制备方法与应用,所述钴铌氧簇为有机‑无机杂化的钴铌氧簇晶态材料,所述钴铌氧簇晶态材料的化学式为Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O;取0.458 g K7HNb6O19·13H2O(0.33 mmol)溶于8 mL水中;另取0.848g砷酸钠Na3AsO4,0.352 g NaCl,0.246 g六水合三氯化钴CoCl3·6H2O和1.4 mL乙二胺加入K7HNb6O19·13H2O水溶液中;搅拌2.5小时,转移至聚四氟乙烯反应釜中,套上外壳;在150℃反应4天,之后冷却至室温得到浅红色块状晶体,该晶体即Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
Description
技术领域
本发明属于多铌氧酸盐的合成技术领域,具体涉及一种钴铌氧簇及其制备方法与应用。
背景技术
能源问题是人类面临的问题之一,利用太阳能光解水制备氧气是一种很有前景的途径之一,多铌氧酸盐具有与半导体氧化物相似的电子属性,因此成为优异的光催化候选者。
过渡金属参与配位有助于调整材料的能带结构,因此过渡金属参与构筑的铌氧簇的合成是新型光催化剂的研究热点。
然而,合成多铌氧酸盐的可溶性前驱体较少,目前主要是[Nb6O19]8-,而该阴离子只能在强碱性环境下存在,过渡金属在此环境下往往易形成沉淀,因此铌氧簇过渡金属衍生物的合成极具有挑战性。
发明内容
解决的技术问题:
本申请针对现有技术的不足,解决了目前[Nb6O19]8-只能在强碱性环境下存在,过渡金属在此环境下往往易形成沉淀等技术问题,提供了一种钴铌氧簇及其制备方法与应用,具有光催化产氧催化剂,该化合物在pH=9的缓冲溶液中展现出较好的光催化产氧性能。
技术方案:
为实现上述目的,本申请通过以下技术方案予以实现:
一种钴铌氧簇,所述钴铌氧簇为有机-无机杂化的钴铌氧簇晶态材料,所述钴铌氧簇晶态材料的化学式为Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
进一步地,所述钴铌氧簇晶态材料属于正交晶系,空间群是Cmmm,晶胞参数是:
一种钴铌氧簇的制备方法,包括以下步骤:
第一步:取0.458g K7HNb6O19·13H2O(0.33mmol)溶于8mL水中;
第二步:另取0-0.848g砷酸钠Na3AsO4,0.352g NaCl,0.246g六水合三氯化钴CoCl3·6H2O和1.4mL乙二胺加入K7HNb6O19·13H2O水溶液中;
第三步:搅拌2.5小时,转移至聚四氟乙烯反应釜中,套上外壳;
第四步:在150℃反应4天,之后冷却至室温得到浅红色块状晶体,该晶体即Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
本申请还公开了所述钴铌氧簇在太阳能光解水制备氧气中的应用。
上述一种钴铌氧簇的制备方法的工作原理在于:为解决[Nb6O19]8-与过渡金属Co2+离子不相容的溶液性质,在合成过程中加入了乙二胺配体,其优先与金属配位,对过渡金属进行保护,以防在碱性条件下水解,钴离子多余的配位点进一步与铌氧簇中氧原子配位,形成有机-无机杂化钴铌氧簇。
有益效果:
本申请提供了一种钴铌氧簇及其制备方法与应用,与现有技术相比,具备以下有益效果:
1.通过本发明制得的钴铌氧簇,展现出光催化产氧的性能。
2.合成步骤少、操作简单、用料价格便宜,号召国家倡导的节能减排的思想。
附图说明
图1为本申请化合物c方向上的二维结构图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,等价形式改动或修改同样落于本申请的权利要求书所限定的范围。
以下实施例中en是指乙二胺。K7HNb6O19·13H2O是根据文献制备(InorganicChemistry,1979,18,93-103),其他是通过阿拉丁购买。
实施例1:
一种钴铌氧簇,所述钴铌氧簇为有机-无机杂化的钴铌氧簇晶态材料,所述钴铌氧簇晶态材料的化学式为Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
一种钴铌氧簇的制备方法,步骤为:
第一步:取0.458g K7HNb6O19·13H2O(0.33mmol)溶于8mL水中;
第二步:另取0.848g砷酸钠Na3AsO4,0.352gNaCl,0.246g六水合三氯化钴CoCl3·6H2O和1.4mL乙二胺加入K7HNb6O19·13H2O水溶液中;
第三步:搅拌2.5小时,转移至聚四氟乙烯反应釜中,套上外壳;
第四步:在150℃反应4天,之后冷却至室温得到浅红色块状晶体,该晶体即Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
实施例2:
本实施例的一种钴铌氧簇,所述钴铌氧簇为有机-无机杂化的钴铌氧簇晶态材料,所述钴铌氧簇晶态材料的化学式为Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
一种钴铌氧簇的制备方法,步骤为:
第一步:取0.458g K7HNb6O19·13H2O(0.33mmol)溶于8mL水中;
第二步:另取0.352g NaCl,0.246g六水合三氯化钴CoCl3·6H2O和1.4mL乙二胺加入K7HNb6O19·13H2O水溶液中;
第三步:搅拌2.5小时,转移至聚四氟乙烯反应釜中,套上外壳;
第四步:在150℃反应4天,之后冷却至室温得到浅红色块状晶体,该晶体即Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
测试例1
分别在实施例1和实施例2中制备得到的晶体中选取优质的单晶用于结构测定,具体如下:
在296K下用BrukerAPEX-II CCD以及在150K下用布鲁克Bruker D8 VENTUREPHOTON II单晶衍射仪对单晶进行测试并收集全部衍射数据,辐射源为石墨单色器的Mo Kα射线 水分子上的氢原子坐标通过差值Fourier合成法得到,所有非氢原子坐标通过直接法得到、并通过各向异性热参数修正以及矩阵最小二乘法优化,氢原子直接加到分子式中。晶体学数据和结构参数见表1。
表1
实施例1和2得到的晶体数据几乎一样。
测试例2
将10μM晶体材料,1.0mM[Ru(bpy)3]Cl2,5.0mM Na2S2O8,pH 9.080mM硼酸钠缓冲溶液,总体积为15mL,加入到单口圆底烧瓶中,反应前,向圆底烧瓶中通入氩气20min,使烧瓶中的空气被氩气置换完全,磁力搅拌使其充分接触均匀,之后采用LED灯(λ≥420nm)光照,采用气相色谱分析计算氧气的量。
表2样品光催化产氧测试结果
以上所述的具体实施例,对本发明的目的、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种用于太阳能光解水制备氧气的钴铌氧簇的制备方法,其特征在于:所述钴铌氧簇为有机-无机杂化的钴铌氧簇晶态材料,所述钴铌氧簇晶态材料的化学式为Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O,制备方法包括以下步骤:
第一步:取0.458 g K7HNb6O19·13H2O 0.33 mmol溶于8 mL水中;
第二步: 另取0-0.848g砷酸钠Na3AsO4, 0.352 g NaCl, 0.246 g 六水合三氯化钴CoCl3·6H2O 和 1.4 mL 乙二胺加入K7HNb6O19·13H2O水溶液中;
第三步: 搅拌2.5小时,转移至聚四氟乙烯反应釜中,套上外壳;
第四步: 在150℃反应4天,之后冷却至室温得到浅红色块状晶体,该晶体即Na3[Nb6O19{Co(en)}2Co0.5(en)]·14H2O。
2.根据权利要求1所述用于太阳能光解水制备氧气的钴铌氧簇的制备方法制得的一种钴铌氧簇,其特征在于:所述钴铌氧簇晶态材料属于正交晶系,空间群是Cmmm。
3.一种权利要求1所述用于太阳能光解水制备氧气的钴铌氧簇的制备方法制得的钴铌氧簇在太阳能光解水制备氧气中的应用。
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