CN113788957A - 一种含硫金属有机配位聚合物材料的制备及其光催化制氢应用 - Google Patents
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- 239000013256 coordination polymer Substances 0.000 title claims abstract description 22
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 17
- 239000001257 hydrogen Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 15
- 239000011593 sulfur Substances 0.000 title claims abstract description 15
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- 239000002184 metal Substances 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- CUJPFPXNDSIBPG-UHFFFAOYSA-N 1,3-propanediyl Chemical group [CH2]C[CH2] CUJPFPXNDSIBPG-UHFFFAOYSA-N 0.000 claims description 8
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- WHMDPDGBKYUEMW-UHFFFAOYSA-N pyridine-2-thiol Chemical compound SC1=CC=CC=N1 WHMDPDGBKYUEMW-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
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- 238000003756 stirring Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical group Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
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- YQGOJNYOYNNSMM-UHFFFAOYSA-N eosin Chemical compound [Na+].OC(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C(O)=C(Br)C=C21 YQGOJNYOYNNSMM-UHFFFAOYSA-N 0.000 description 1
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- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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Abstract
本申请涉及一种新型含硫金属有机配位聚合物材料的制备方法及其在光催化制氢方面的应用。其化学式为[Ni(4,4'‑dipy)(PySH)2]n，可通过水热法得到蓝色晶体，正交晶系，空间群为P 212121,晶胞参数a=9.784(2)Å，b=17.742(4)Å，c=26.376(5)Å，α=90°，β=90°，γ=90°，Z=2，晶胞体积V=4578.4(16)Å3。该配位聚合物材料在可见光照射下表现出良好的制氢性能。
Description
技术领域
本发明属于配位聚合物材料领域，具体涉及一种含硫金属有机配位聚合物材料的制备及其在光催化制氢领域的应用。
背景技术
随着经济的快速发展，能源和环境问题已成为世界各国共同关注的焦点。光催化制氢反应，能够有效利用太阳能将水资源转化为清洁的氢能源，是解决能源危机和环境问题的有效方法之一。金属有机配位聚合物由于结构精确、易于设计调控等优点受到了光催化制氢领域的广泛关注。部分基于非贵金属的配位聚合物材料被设计作为催化剂应用于光催化制氢反应中，但通常存在稳定性不高、效率偏低等问题。
含硫配体的配位模式多样，易与过渡金属离子Ni2+配位组装出结构新颖的配位聚合物，并且通常在水溶液中表现出比较高的稳定性。另外，引入活性较高的NiS催化位点，有助于提升催化活性。因此，本申请选取含硫配体与非贵金属离子Ni2+制备新型金属有机配位聚合物材料用于光催化制氢反应。
发明内容
本发明提供一种含硫金属有机配位聚合物材料的制备及其在光催化制氢领域的应用。
所述含硫金属有机配位聚合物材料的化学式为[Ni(4,4'-dipy)(PySH)2]n，正交晶系，空间群为P 212121, 晶胞参数a = 9.784(2) Å，b = 17.742(4) Å，c = 26.376(5) Å，α=90°，β= 90°，γ= 90°，Z = 2, 晶胞体积V = 4578.4(16) Å3。其中，4,4'-dipy为4,4'-(1,3-丙二基)双吡啶，PySH为2-巯基吡啶。
所述含硫金属有机配位聚合物材料[Ni(4,4'-dipy)(PySH)2]n的制备方法，通过水热法制备，将2-巯基吡啶、4,4'-(1,3-丙二基)双吡啶、镍源、碱源和水混合搅拌均匀后，于特定温度下晶化得到。
其中，2-巯基吡啶、4,4'-(1,3-丙二基)双吡啶、镍源、碱源的摩尔比例为0.9~1:0.45~0.5:0.45~0.5:1，镍源为NiCl2•6H2O，碱源为氢氧化钾。水热反应的条件为通过37.5℃/h的升温速率由室温升至180℃，再以0.625℃/h的速率由180℃降至150℃，然后以2.5℃/h的速率由150℃降至室温。
本发明提供了上述材料[Ni(4,4'-dipy)(PySH)2]n在光催化制氢领域的应用，具体是在光敏剂和牺牲剂的共同作用下，该材料在可见光照射下表现出良好的催化制氢性能。
本申请所述技术方案的有益效果为：
本发明通过简便的制备方法，得到了一种结构新颖的金属有机配位聚合物材料[Ni(4,4'-dipy)(PySH)2]n。在光敏剂和牺牲剂的共同作用下，该金属有机配位聚合物材料在可见光照射下表现出良好的催化制氢性能。
附图说明
图1是本发明实施例1所制备的金属有机配位聚合物材料[Ni(4,4'-dipy)(PySH)2]n的结构基元示意图，该晶体通过4,4'-(1,3-丙二基)双吡啶配体两端的N原子与Ni配位并无限延伸。
图2是本发明实施例1所制备的金属有机配位聚合物材料[Ni(4,4'-dipy)(PySH)2]n的X射线粉末衍射图谱。其中a是对解析出的晶体结构进行拟合得到的衍射图谱；b是将样品磨碎后进行X射线粉末衍射得到的图谱。
图3 是本发明实施例1所制备的金属有机配位聚合物材料[Ni(4，4'-dipy)(PySH)2]n在光敏剂和牺牲剂存在下的光催化制氢性能。
具体实施方式
实施例1 采用水热法合成[Ni(4,4'-dipy)(PySH)2]n晶体
按照一定摩尔比称取2-巯基吡啶、4,4'-(1,3-丙二基)双吡啶、NiCl2•6H2O和氢氧化钾于水热反应罐中，加入8mL去离子水，搅拌后密封加热，水热反应的条件为通过37.5℃/h的升温速率由室温升至180℃，再以0.625℃/h的速率由180℃降至150℃，然后以2.5℃/h的速率由150℃降至室温。反应结束后，用去离子水和乙醇交替洗涤，得到蓝色晶体。各原料的配比和样品编号如表1所示。
表1 样品[Ni(4,4'-dipy)(PySH)2]n的合成条件
实施例2 光催化制氢性能研究
称取10mg[Ni(4,4'-dipy)(PySH)2]n加入到含有5mM曙红（光敏剂）及15%TEOA（牺牲剂）的水溶液中，调节溶液pH=8.5。而后将溶液转移至反应瓶中进行光催化反应，表现出的光催化制氢性能如图3所示。
以上所述，仅是本发明的几个实施例，并非对本发明做任何形式的限制，虽然本发明以较佳实施例揭示如上，然而并非用以限制本发明，任何熟悉本专业的技术人员，在不脱离本发明技术方案的范围内，利用上述揭示的技术内容做出些许的变动或修饰均等同于等效实施案例，均属于技术方案范围内。
Claims (10)
1.一种含硫金属有机配位聚合物材料，其特征在于，其化学式为[Ni(4,4'-dipy)(PySH)2]n，正交晶系，空间群为P 212121，晶胞参数a = 9.784(2) Å，b = 17.742(4) Å，c =26.376(5) Å，α= 90°，β= 90°，γ= 90°，Z = 2, 晶胞体积V = 4578.4(16) Å3；其中，4,4'-dipy为4,4'-(1,3-丙二基)双吡啶，PySH为2-巯基吡啶，n为正整数。
2.如权利要求1所述含硫金属有机配位聚合物材料的合成方法，其特征在于，通过将2-巯基吡啶、4,4'-(1,3-丙二基)双吡啶、镍源和碱源称量后，加入去离子水，搅拌后密封在反应釜中，进行水热反应；反应结束后，用去离子水和乙醇洗涤，得到蓝色目标晶体，即含硫金属有机配位聚合物材料。
3.根据权利要求2所述的合成方法，其特征在于，2-巯基吡啶、4,4'-(1,3-丙二基)双吡啶、镍源和碱源按照摩尔比0.9~1:0.45~0.5:0.45~0.5:1配料。
4.根据权利要求2所述的合成方法，其特征在于，所述镍源为NiCl2•6H2O。
5.根据权利要求2所述的合成方法，其特征在于，所述的碱源为氢氧化钾。
6.根据权利要求2所述的合成方法，其特征在于，去离子水的加入量为8mL。
7.根据权利要求2所述的合成方法，其特征在于，水热反应的条件为由室温升温至180℃，再由180℃降温至150℃，然后二次降温，由150℃降至室温。
8.根据权利要求7所述的合成方法，其特征在于，升温速率为37.5℃/h，首次降温速率为0.625℃/h。
9.根据权利要求7所述的合成方法，其特征在于，二次降温速率为2.5℃/h。
10.一种权利要求1所述含硫金属有机配位聚合物材料在光催化制氢反应中的应用。
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| CN108997587A (zh) * | 2018-06-21 | 2018-12-14 | 三峡大学 | 一种用于电解水制氢反应的金属有机框架材料及其纳米片材料的制备方法 |
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| CN116444806A (zh) * | 2023-02-24 | 2023-07-18 | 福州大学 | 一种镍硫配位聚合物及其制备与应用 |
| CN116444806B (zh) * | 2023-02-24 | 2024-08-02 | 福州大学 | 一种镍硫配位聚合物及其制备与应用 |
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