CN113368902A - 一种Fe2Co-MOFs装载离子液体CO2还原光催化剂的制备 - Google Patents
一种Fe2Co-MOFs装载离子液体CO2还原光催化剂的制备 Download PDFInfo
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Abstract
本发明属于金属‑有机框架材料催化剂领域，具体为一种Fe2Co‑MOFs（PCN‑250‑Fe2Co）装载离子液体（ILs）CO2还原光催化剂的制备,它涉及一种CO2还原光催化剂的制备方法。本发明的主要目的是要解决现有的PCN‑250‑Fe2Co材料吸附CO2能力弱，光催化CO2还原活性低的缺点。方法：一、利用水热反应制备PCN‑250‑Fe2Co金属有机框架材料；二、通过机械法将离子液体装载到PCN‑250‑Fe2Co孔道中制备得到CO2还原光催化剂ILs@PCN‑250‑Fe2Co。本发明制备的ILs@PCN‑250‑Fe2Co在300W氙灯可见光的波长范围照射下CO2还原为CO速率最高可以达到501.8μmolg‑ 1h‑1。本发明可以获得一种PCN‑250‑Fe2Co装载ILs光催化CO2还原催化剂的制备方法。
Description
技术领域
本发明属于金属-有机框架材料催化剂领域，具体涉及一种ILs@PCN-250-Fe2Co复合材料的制备及光催化CO2还原为CO。
背景技术
第二次工业革命以来，化石燃料被广泛的开发和利用，导致了空气中温室气体（以CO2为主）浓度越来越高，由此引发一系列的能源问题与环境问题。受到植物光合作用启发，利用太阳光将二氧化碳还原为有价值的含碳燃料引起科学家们的广泛关注。因此，制备一些结构稳定，二氧化碳吸附能力强，具有有效的电子传输性能的光催化剂具有十分光明的前景。
金属有机框架(MOFs)因其多孔结构、优异的比表面积、可调的孔道结构等优点，在不同领域都有广泛的应用，如荧光、传感、载药、气体储存、催化等。我们希望利用具有大比表面积、高稳定性和优异催化活性的MOFs材料PCN-250-Fe2Co作为光催化剂载体，实现高效人工光合成CO2还原为CO等含碳燃料，但是单独的PCN-250-Fe2Co材料在光催化进程中对于CO2的吸附量较差，阻碍了其催化效果。而咪唑类离子液体（ILs）能够富集CO2，将ILs与PCN-250-Fe2Co材料复合可以有效增强PCN-250-Fe2Co材料对CO2的吸附能力。因此我们将PCN-250-Fe2Co与ILs两相结合，构筑具有主客体协同催化作用的光催化剂，大大提高PCN-250-Fe2Co材料的人工光催化CO2还原活性的目的。
发明内容
本发明的目的在于解决现有的纯MOFs材料对CO2吸附能力较弱，制约光催化CO2还原能力的问题，构筑的具有主客体协同作用的ILs@PCN-250-Fe2Co有良好的二氧化碳吸附和活化能力，能够光催化CO2还原为CO，可作为光催化剂。
本发明的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备方法是按以下步骤完成的：
一、将PCN-250-Fe2Co置于无水乙醇中，在超声频率为35~45KHz超声分散20 min~30 min后转移到磁力搅拌器上，在搅拌速度为350r/min~400r/min下搅拌1h~2h；然后缓慢滴加ILs，继续搅拌8h~10h，得到ILs@PCN-250-Fe2Co复合材料；
步骤一中的制备好的PCN-250-Fe2Co的质量和无水乙醇体积比为1mg：0.1mL~1mg：0.2mL；
步骤一中所述的ILs加入的量为5~6μL；
二、将步骤一中得到的ILs@PCN-250-Fe2Co复合材料均匀的涂覆在玻璃片上，利用红外灯将无水乙醇烘干，得到ILs@PCN-250-Fe2Co薄膜作为CO2还原光催化剂；
步骤二中的玻璃片为直径3~5cm，厚度2~3mm的圆形玻璃片，红外灯照射时间为2~3min；
光催化CO2气固还原活性测试过程如下：将步骤二中所得到的自支撑膜放入气固反应器中。然后加入少量的水并用高纯CO2气体吹扫30 min，直至将反应器中空气充分排除后将反应器密封。该反应体系利用300 W Xe灯在可见光条件下照射。每小时采集一次气体样本，通过GC7920在线气相色谱仪中的FID2检测器的检测CO气体。
本发明的有益效果为：
本发明通过制备将ILs装载在PCN-250-Fe2Co的孔道中，构筑了具有主客体协同作用的ILs@PCN-250-Fe2Co复合材料，解决了PCN-250-Fe2Co对二氧化碳吸附能力差的缺点，从而提高了光催化CO2还原性能，本发明制备的ILs@PCN-250-Fe2Co材料利用300 W Xe灯在可见光范围内照射，产率达到501.8μmolg-1h-1~524.3μmolg-1h-1，比单独的PCN-250-Fe2Co提高了10倍以上。
附图说明
图1为ILs@PCN-250-Fe2Co的合成路线图；
图2为ILs@PCN-250-Fe2Co的X射线粉末衍射图；
图3为ILs@PCN-250-Fe2Co的扫描电镜图；
图4为ILs@PCN-250-Fe2Co的光催化CO2还原为CO性能测试图。
具体实施方式
实施例1：本实施方式的一种PCN-250-Fe2Co装载ILs光催化还原二氧化碳催化剂的制备方法是按以下步骤完成的：
步骤一、将100 mg 3, 3', 5, 5'-偶氮苯四酸，150 mg Fe2Co金属簇和4 mL浓度为3mol/L乙酸分别置于30mL N,N-二甲基甲酰胺（DMF）中，400r/min的转速搅拌1h后转移到高压反应釜中。混合物在140°C的烘箱中加热2 h，反应后待反应釜冷却到室温，8000r/min离心10min收集反应产物并用DMF洗涤3次，丙酮洗涤3次，并用丙酮浸泡24h，最后在120 ℃下真空干燥12 h得到200mgPCN-250-Fe2Co；
步骤二、将步骤一中得到的10mgPCN-250-Fe2Co分散到1mL乙醇中，超声分散30min后转移到磁力搅拌器上在搅拌速度为400r/min下搅拌2h；然后滴加5μL ILs，继续搅拌8h，然后将得到ILs@PCN-250-Fe2Co复合材料均匀的涂覆在玻璃片上，利用红外灯将无水乙醇烘干，得到ILs@PCN-250-Fe2Co薄膜作为CO2还原光催化剂。
PCN-250-Fe2Co装载ILs光催化还原CO2催化剂材料的表征及性能检测。
图1为实施例1的合成步骤流程。
图2对实施例1得到的ILs@PCN-250-Fe2Co光催化剂材料进行X-射线粉末衍射（PXRD）检测，得到如图2所示：1为 PCN-250-Fe2Co的标准模拟峰；2为实施例1制备的PCN-250-Fe2Co的XRD图，3为实施例1制备的PCN-250-Fe2Co装载ILsCO2还原光催化剂材料的XRD图；所得的ILs@PCN-250-Fe2Co复合材料的X-射线衍射峰与标准模拟峰均能吻合。这些结果证明装载ILs的PCN-250-Fe2Co均保持原有的晶型。
图3为实施例1得到的ILs@PCN-250-Fe2Co和PCN-250-Fe2Co的扫描电镜图，a)和b)可以看出纯 PCN-250-Fe2Co表现出粒径约为15μm的多面体形态；ILs@PCN-250-Fe2Co复合材料呈片状堆积的形貌，片状的尺寸在1~5μm。c)和d)是ILs@PCN-250-Fe2Co复合材料制备成薄膜后断口处的形貌图，薄膜的厚度约为20μm，且表面厚度均匀。以上结果表明，ILs的加入会对PCN-250-Fe2Co的形貌产生明显影响，因此片状形貌的复合材料涂覆在玻璃片上，可以更好的被制备成自支撑膜。
对实施例1得到的ILs@PCN-250-Fe2Co光催化剂材料进行光催化CO生成速率图，得到PCN-250-Fe2Co装载ILs二氧化碳还原为一氧化碳的速率图，本发明的光催化材料最高一氧化碳产率可以达到501.8μmolg-1h-1。
本具体实施所得的ILs@PCN-250-Fe2Co光催化剂材料，有良好的二氧化碳还原能力，能够光催化二氧化碳还原为一氧化碳，可作为光催化剂。
Claims (6)
1.一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备方法，其特征在于该方法按以下步骤进行：
步骤一、ILs@PCN-250-Fe2Co的制备：将PCN-250-Fe2Co置于无水乙醇中，超声一定时间后转移到磁力搅拌器上以一定的转速搅拌1h~2h；然后缓慢滴加ILs，继续搅拌8h~10h，得到ILs@PCN-250-Fe2Co复合材料；
步骤二、将步骤一中得到的ILs@PCN-250-Fe2Co复合材料均匀的涂覆在玻璃片上，利用红外灯将无水乙醇烘干，得到ILs@PCN-250-Fe2Co薄膜作为CO2还原光催化剂。
2.根据权利要求1所述的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备，其特征在于步骤一中所述超声频率为35~45KHz，超声时间为20 min~30 min。
3.根据权利要求1所述的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备，其特征在于步骤一中所述搅拌速度为350r/min~400r/min。
4.根据权利要求1所述的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备，其特征在于步骤一中所述PCN-250-Fe2Co的质量和无水乙醇的体积比为1mg：0.1mL~1mg：0.2mL。
5.根据权利要求1所述的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备方法，其特征在于步骤一中所述PCN-250-Fe2Co的质量和ILs的体积比为1mg：0.5μL~1mg：0.6μL。
6.根据权利要求1所述的一种PCN-250-Fe2Co装载ILs光催化CO2还原催化剂的制备方法，其特征在于步骤二中所述的红外灯功率为100W，照射时间为2min ~3min。
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