CN112138691A - 一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法 - Google Patents
一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法，包括以下步骤(1)称取0.82g 2‑甲基咪唑，一定量导电炭黑和一定量石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀；(2)0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀；(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h；用甲醇，乙醇进行离心处理，干燥处理，生成Co‑MOF‑C纳米粒子；(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC‑2催化剂。本发明方法制得的含N,C,P层包裹的CoP纳米析氢电催化剂具有较高的电催化析氢活性和稳定性。
Description
技术领域
本发明涉及一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法，具体涉及一种利用ZIF-67合成过程中XC-72R和石墨炔的协同效应经磷化合成N,C,P层包裹的CoP纳米高性能析氢催化剂的方法，所得到的石墨炔增强的含N,C,P层包裹的CoP纳米高性能析氢催化剂具有析氢催化活性高，导电性好，酸性条件下稳定性高等优点。
背景技术
近年来，由于能源短缺和环境污染，氢能源由于其绿色，环保，来源广泛等优点被认为是最有前途的绿色燃料。电解水制氢是目前最环保无污染的制氢方法。高效的催化剂可以降低过电位，促进氢的释放反应。众所周知，铂(Pt)作为最有效的析氢催化剂，由于其成本高，含量少的缺点而不能被广泛应用于析氢反应中。因此，寻找低成本，高效催化的催化剂具有重要意义。
目前，文献中报道的低成本、高催化效用的催化剂主要是利用过渡金属材料铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、钼(Mo)、钨(W)等和给金属材料硼(B)、碳(C)、氮(N)、氧(O)、硫(S)、磷(P)、硅(Si)等制备合成。近年来，过渡金属磷化物(TMPs)由于其低成本，良好的化学稳定性和宽广的电催化剂HER催化活性的PH范围而备受关注。与其他过渡金属磷酸盐相比，例如铁，铜，镍和钨，CoP似乎更受人们的关注，因为具有更强电负性的磷原子与Co结合，可捕获金属原子中的电子并充当载体。特别是从金属有机骨架(MOF)，例如ZIF-67等。MOF具有开放的晶体结构，出色的孔隙率，结构柔韧性和可调功能。
对于石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂而言，XC-72R和石墨炔的协同效应，这在设计电化学析氢反应方面具有明显优势。到目前为止，通过利用ZIF-67合成过程中XC-72R和石墨炔的协同效应经磷化合成N,C,P层包裹的CoP纳米高性能析氢催化剂的方法未见报道。
发明内容
本发明涉及一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法，具体涉及一种利用ZIF-67合成过程中XC-72R和石墨炔的协同效应经磷化合成N,C,P层包裹的CoP纳米高性能析氢催化剂的方法，所得到的石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂具有析氢催化活性高，导电性好，酸性条件下稳定性高等优点。
本发明先通过ZIF-67合成过程中XC-72R和石墨炔的协同效应经磷化合成N,C,P层包裹的CoP纳米高性能析氢催化剂，其具体制备工艺为：
称取(1)0.82g 2-甲基咪唑，一定量导电炭黑和一定量石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-C纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC-2催化剂。
本发明所涉及产品工艺简单易实现，产品质量稳定，反应参数容易控制、安全可靠等优点；所制备的N,C,P层包裹的CoP纳米高性能析氢催化剂具有析氢催化活性高，导电性好，酸性条件下稳定性高等优点。
附图说明
图1中a为实施例1制备的Co-MOF-XC-72R，b为实施例5制备的Co-MOF-GDY，c为实施例3制备的Co-MOF-C，d为实施例3制备的CoP@NPC-2催化剂的扫描电子显微镜图像。
图2为实施例3制备的电极材料的X射线衍射图谱。
图3为实施例1-6制备的电极材料和参比催化剂20％Pt/C的线性扫描伏安曲线，
具体实施方式
实施例1
(1)称取0.82g 2-甲基咪唑，15mg导电炭黑XC-72R加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-XC-72R纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC-0催化剂。
实施例2
(1)称取0.82g 2-甲基咪唑，15mg导电炭黑XC-72R和1mg石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-C纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC-1催化剂。
实施例3
(1)称取0.82g 2-甲基咪唑，15mg导电炭黑XC-72R和2mg石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-C纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC-2催化剂。
实施例4
(1)称取0.82g 2-甲基咪唑，15mg导电炭黑XC-72R和3mg石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-C纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NPC-3催化剂。
实施例5
(1)称取0.82g 2-甲基咪唑，2mg石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-GDY纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP@NP-2催化剂。
实施例6
(1)称取0.82g 2-甲基咪唑加入到20mL甲醇溶液中，超声处理直至混合均匀。(2)称取0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀。(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h。用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF纳米粒子。(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到CoP催化剂。
从本发明制得的石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂测试结果来看，本发明所得到石墨炔增强的N,C,P层包裹的CoP纳米颗粒具有析氢活性高，导电性好，酸性条件下稳定性高等优点。
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (3)
1.本发明涉及一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电催化剂的制备方法，具体涉及一种合成ZIF-67过程中掺杂XC-72R和石墨炔再经过磷化处理得到石墨炔增强的N,C,P层包裹的CoP纳米颗粒高性能析氢催化剂的方法，合成方法为：称取(1)0.82g 2-甲基咪唑，一定量导电炭黑和一定量石墨炔(GDY)加入到20mL甲醇溶液中，超声处理直至混合均匀；(2)0.291g六水合硝酸钴加入到20mL甲醇中，超声至混合均匀；(3)将两种甲醇溶液混合，60℃水浴剧烈搅拌5min，静置20h；用甲醇，乙醇进行离心处理，干燥处理，生成Co-MOF-C纳米粒子；(4)在管式炉中进行磷化处理，升温速率为2℃/min，于350℃保温2h，得到一种石墨炔增强的含N,C,P层包裹的CoP纳米颗粒催化剂。
2.根据权利要求1所述的制备方法，其特征在于步骤(1)中导电炭黑的质量为0，15mg，石墨炔的质量为0-3mg。
3.根据权利要求1所述的制备方法，所得到石墨炔增强的含N,C,P层包裹的CoP纳米颗粒电析氢催化剂，电化学测试表明：其电流密度达到10mA·cm-2时，过电位仅有144mV，Tafel斜率较小为67mV·dec-1。
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