CN110586196B - 一种FeOOH@Ni-BDC电解水催化剂的制备方法 - Google Patents
一种FeOOH@Ni-BDC电解水催化剂的制备方法 Download PDFInfo
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- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005868 electrolysis reaction Methods 0.000 title description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 34
- 239000004744 fabric Substances 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 24
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002135 nanosheet Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims abstract description 6
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000001632 sodium acetate Substances 0.000 claims abstract description 6
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 6
- 238000004070 electrodeposition Methods 0.000 claims abstract description 4
- 239000003792 electrolyte Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000004729 solvothermal method Methods 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 239000008204 material by function Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 230000003197 catalytic effect Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明涉及一种碳布负载的FeOOH@Ni‑BDC复合电解水催化剂及其制备方法，属于新型无机纳米功能材料制备技术领域。本发明以碳布负载的FeOOH纳米片阵列为模板，通过水热法制备在其上包覆Ni‑BDC形成FeOOH@Ni‑BDC复合催化剂。具体步骤如下：首先通过电沉积法以硫酸亚铁铵,醋酸钠和硫酸钠混合溶液为电解液制得碳布负载的FeOOH纳米片阵列为模板；进一步在溶剂热条件下使用氯化镍和对苯二甲酸形成金属有机骨架并包覆在FeOOH纳米片上制得FeOOH@Ni‑BDC复合电解水催化剂。
Description
技术领域
本发明涉及一种FeOOH@Ni-BDC复合电解水催化剂及其制备方法，属于新型无机纳米功能材料技术领域。
背景技术
近年来，能源短缺及环境污染等问题日益引起人们的高度重视，发展新型清洁能源技术迫在眉睫。电解水作为一种有效的产氢方法受到了广泛的关注。但是，从化学热力学角度来说，水分解过程属于非自发化学反应且需要额外的过电势才驱动其进行，因而发展高效稳定的催化剂对于提高电解水效率、降低电能消耗具有重要的意义。目前，对电解水反应催化性能最好的催化剂大多是铂、铑、铱等贵金属材料，价格昂贵且来源稀少，严重制约了其广泛利用。科学家近来的研究成果表明，以铁、钴、镍为代表的过渡金属基催化剂，如氧化镍、硫化钴等，也就有优异的电解水性能，且此类材料价格低廉，适宜大规模应用。但是，此类催化剂的制备往往需要高温加热处理，产物不可避免的会发生一定程度的聚集，从而降低催化活性。同时高温加热的过程还具有耗能较高、反应过程比较复杂，无法精确定量控制等缺点。
羟基氧化铁(FeOOH)因其活性位点暴露、价格低廉等优点而常被用于制备电解水催化剂。但是FeOOH导电性较差、比表面积小且传质效率低，因此催化效果不够理想。金属有机骨架具有开放式的结构、高比表面积等特点。将FeOOH和金属有机骨架相结合，可以发挥二者协调效应，实现优势互补，制备性能优良的复合电解水催化剂。本发明将一种由氯化镍和对苯二甲酸形成的金属有机骨架(Ni-BDC)和FeOOH相结合，利用二者的特点，发展了一种成本低廉、简便易行、低能耗的复合电解水催化剂的制备方法，制备了具有优异催化性能的FeOOH@Ni-BDC复合电解水催化剂。
发明内容
本发明的目的在于提供一种成本低廉、简便易行的FeOOH@Ni-BDC复合电解水催化剂的制备方法。本发明提供的这种制备方法，工艺简单，成本低廉，且所制备的FeOOH@Ni-BDC具有优异的电解水催化性能，具有较高的实际应用价值。
本发明的目的是通过以下技术方案实现的，一种FeOOH@Ni-BDC复合电解水催化剂的制备方法，包括以下步骤：
1）将提前裁剪好的碳布(2×1 cm)用5%盐酸、丙酮和去离子水分别超声15分钟；
2）将步骤1所得碳布浸入到含有一定浓度的硫酸亚铁铵, 醋酸钠和硫酸钠混合溶液中，在一定的电流强度下进行电沉积制备碳布负载的FeOOH纳米片阵列；
3）在水热反应釜中加入一定摩尔比的氯化镍和对苯二甲酸，并添加一定体积N,N’-二甲基甲酰胺，然后搅拌溶解；
4）将步骤2所得碳布负载的FeOOH加入到步骤3所得反应釜溶液中，然后放置到烘箱中加热得到碳布负载的FeOOH@Ni-BDC复合电解水催化剂。
本发明的有益效果：
（1）本发明提供了一种新型FeOOH@Ni-BDC复合电解水催化剂的制备方法，即首先通过简单的电沉积制备碳布负载的FeOOH纳米片阵列，再继续再以碳布负载的FeOOH阵列为模板，通过水热法制备FeOOH@Ni-BDC阵列。制备方法简单易操作，不需要特殊的设备，成本低廉且适于大规模制备，可以满足实际应用的需求；
（2）本发明制备的产物为碳布负载FeOOH@Ni-BDC纳米片阵列，产物形貌规则、尺寸均匀，以碳布作为载体负载催化剂利于实际应用；
（3）本发明制备的FeOOH@Ni-BDC复合电解水催化剂有效的结合两种组份的优点，利用二者的协同效应得到了具有优异催化性能及良好稳定性的催化剂；
（4）本发明的制备仅需实验室常用的普通设备，不需专用设备，工艺过程简便易行。
附图说明
图1为本发明方法所制备的FeOOH@Ni-BDC纳米片阵列复合电解水催化剂用美国FEI QUANTA FEG250扫描电子显微镜观察后拍摄的扫描电镜（SEM）照片；
图2是本发明方法所制备的FeOOH@Ni-BDC纳米片阵列复合电解水催化剂的X射线衍射（XRD）图。
具体实施方式
下面通过具体实施实例并结合附图对本发明的内容作进一步详细说明，但这些实施例并不限制本发明的保护范围。
实施例1
将提前处理好的碳布浸入到一定浓度的硫酸亚铁铵(90 mM), 醋酸钠(180 mM)和硫酸钠(90 mM)的混合溶液中，在0.125 mA cm-2的电流强度下电沉积3个小时制备碳布负载的FeOOH纳米片阵列。在水热反应釜中加入1.70毫摩尔的氯化镍，0.55毫摩尔的对苯二甲酸和15毫升N,N’-二甲基甲酰胺，然后在搅拌溶解后将之前所制备的碳布负载的FeOOH加入到反应釜溶液中，然后放置到烘箱中在120摄氏度下加热15小时得到碳布负载的FeOOH@Ni-BDC复合电解水催化剂。
实施例2
将提前处理好的碳布浸入到一定浓度的硫酸亚铁铵(100 mM), 醋酸钠(200 mM)和硫酸钠(100 mM)的混合溶液中，在0.125 mA cm-2的电流强度下电沉积4个小时制备碳布负载的FeOOH纳米片阵列。在水热反应釜中加入1.50毫摩尔的氯化镍，0.50毫摩尔的对苯二甲酸和12毫升N,N’-二甲基甲酰胺，然后在搅拌溶解后将之前所制备的碳布负载的FeOOH加入到反应釜溶液中，然后放置到烘箱中在130摄氏度下加热16小时得到碳布负载的FeOOH@Ni-BDC复合电解水催化剂。
实施例3
将提前处理好的碳布浸入到一定浓度的硫酸亚铁铵(90 mM), 醋酸钠(180 mM)和硫酸钠(90 mM)的混合溶液中，在0.15 mA cm-2的电流强度下电沉积3个小时制备碳布负载的FeOOH纳米片阵列。在水热反应釜中加入1.70毫摩尔的氯化镍，0.6毫摩尔的对苯二甲酸和15毫升N,N’-二甲基甲酰胺，然后在搅拌溶解后将之前所制备的碳布负载的FeOOH加入到反应釜溶液中，然后放置到烘箱中在110摄氏度下加热20小时得到碳布负载的FeOOH@Ni-BDC复合电解水催化剂。
实施例4
使用辰华660D电化学工作站对碳布负载的FeOOH@Ni-BDC复合电解水催化剂电解水催化活性及稳定性进行测试。以铂丝为对电极，银/氯化银为参比电极，碳布负载的FeOOH@Ni-BDC为工作电极，1.0摩尔每升KOH水溶液为电解质溶液。在1.0 至2.0 V电压范围内，以2毫安每秒的扫速进行线性伏安扫描，即可得到其催化电解水产氧的极化曲线。
Claims (3)
1.一种碳布负载的FeOOH@Ni-BDC复合电解水催化剂的制备方法，其特征在于制备方法的步骤如下：
1）采用电沉积法，以硫酸亚铁铵，醋酸钠和硫酸钠混合溶液为电解液制得碳布负载的FeOOH纳米片阵列为模板；
2）在另一反应釜中加入氯化镍、对苯二甲酸和N,N’-二甲基甲酰胺，将步骤1）所得碳布负载的FeOOH纳米片阵列转移至其中，然后通过溶剂热反应制得碳布负载的FeOOH@Ni-BDC复合电解水催化剂。
2.根据权利要求1所述的碳布负载的FeOOH@Ni-BDC复合电解水催化剂的制备方法，其特征在于，所述复合电解水催化剂是以碳布负载的FeOOH纳米片阵列为模板的。
3.根据权利要求1所述的碳布负载的FeOOH@Ni-BDC复合电解水催化剂的制备方法，其特征在于，所述复合电解水催化剂中金属有机骨架是由氯化镍和对苯二甲酸在溶剂热条件下形成的。
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