CN108435252A - 一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法 - Google Patents
一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法 Download PDFInfo
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- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 3
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Abstract
本发明提供一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法，该方法将还原氧化石墨烯（rGO）作为催化剂载体，以导电聚合物多金属氧酸盐聚吡咯钼磷酸盐（(PPy)3PMo12O40）为修饰剂，以氯铂酸为铂源，乙二醇为还原剂制备导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO。该类复合催化剂既具有良好的抗一氧化碳中毒性能又具有良好的导电性，因而对甲醇氧化具有促进作用，是一类具有潜在应用前景的直接甲醇燃料电池催化剂。
Description
技术领域
本发明涉及一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法。
背景技术
由于化石燃料的逐渐枯竭以及环境问题的加剧，促使人们积极寻求可再生能源及清洁能源。直接甲醇燃料电池（DMFCs）由于其燃料易于储存，能量密度高，污染物排放低以及电池结构简单等特点，成为潜在的可持续绿色能源。铂基（Pt基）催化剂是DMFC的优良阳极催化剂，但由于Pt 价格昂贵，储量少，且易受一氧化碳（CO）中毒，使DMFC的实际应用受到阻碍。因此，如何提高Pt催化剂的抗CO中毒性能、稳定性和电催化活性对DMFC的发展至关重要。
多金属氧酸盐（POMs）是由过渡金属和氧形成的一类含有氧桥的多核混合价态化合物，具有独特的结构和性质。Keggin型多金属氧酸盐（如PMo12O40 3−）由于其优良的氧化还原性质可用于一系列催化氧化反应。有研究表明，在DMFC的阳极电催化剂中引入多金属氧酸盐，可充当氧化剂，将中间产物CO转化成无毒的CO2，从而阻止催化剂CO中毒失活。氧化过程如下所示：
CO(g) + H2O(l) + PMo12O40 3−(aq) → CO2(g) + 2H+(aq) + PMo12O40 5−(aq) (1)
此外，多金属氧酸是优秀的无机构筑块，与不同有机体结合，可形成具有新型功能特性的有机-无机杂化多金属氧酸盐材料，兼具有机和无机基块的性能， 衍生出许多单个分子所不具备的新性质。
导电聚合物由许多具有共轭π键聚合的单体组成，具有比表面积大、稳定性强、导电率高等特点，被认为是较为理想的电极材料。在众多导电聚合物中，聚吡咯（PPy）因其高的电导率、氧化还原性能、环境稳定性以及易于制备等优点成为近年来的研究热点。若将聚吡咯作为有机配体与多金属氧酸盐结合制备聚吡咯多金属氧酸盐，可兼具多金属氧酸阴离子与聚吡咯有机阳离子的优点。
因此，将还原氧化石墨烯作为催化剂载体，将导电聚合物多金属氧酸盐作为修饰剂，构筑新型Pt/导电聚合多金属氧酸盐/还原氧化石墨烯复合催化剂材料，可望改善Pt基催化剂的抗CO中毒性能、导电性、稳定性，从而有效提高催化剂的甲醇氧化电催化活性，为DMFC催化剂的开发和应用提供有益借鉴。
发明内容
一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法。
本发明涉及一种导电聚合物多金属氧酸盐复合铂催化剂，其成分为铂/聚吡咯钼磷酸盐/还原氧化石墨烯（(PPy)3PMo12O40），合成步骤包括以下几步。
(1) 0.7mL吡咯置于玛瑙研钵中冷冻1 h，加入研细的过硫酸铵1.5974g，研磨5min，再加入研细的钼磷酸(H3PMo12O40·nH2O) 4.2000 g，混合研磨2 h，得到干爽的黑色粉末，将其放置48 h，用水、乙醇和乙醚洗涤得到成分为聚吡咯钼磷酸盐（(PPy)3PMo12O40）的导电聚合物多金属氧酸盐。
(2) 将0.02 g聚吡咯钼磷酸盐（(PPy)3PMo12O40）加入1 mL N，N-二甲基甲酰胺溶解。
(3) 加入25 mL乙二醇，超声5min混合均匀。
(4) 加入0.04 g氧化石墨，超声分散30min。
(5) 依次加入1 mL 0.05 mol•L-1的氯铂酸（H2PtCl6•6H2O）乙二醇溶液和0.4 mL0.4 mol•L-1的氢氧化钾水溶液，然后磁力搅拌3 h，使其充分混合。
(6) 将步骤(5)的混合溶液于160 ℃反应3 h之后自然冷却至室温，继续搅拌12h。
(7) 用高纯水和丙酮洗涤，60 ℃真空干燥12 h，制得导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO。
附图说明
图1是本发明制备的导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO的高分辨透射电镜照片和粒径分布图，由图1a可看出，以导电聚合物多金属氧酸盐为修饰剂的复合铂催化剂均匀分散于催化剂载体rGO上，由图1b粒径分布图可知Pt粒径约为2.6±0.2 nm。
图2是本发明制备的导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO与20 %商业铂碳（Pt/C）催化剂、铂/还原氧化石墨烯（Pt/rGO）的甲醇氧化循环伏安曲线，由图2可看出，Pt/(PPy)3PMo12O40/rGO的甲醇氧化电催化活性远远高于20 %商业Pt/C催化剂和Pt/rGO，说明修饰剂导电聚合物多金属氧酸盐(PPy)3PMo12O40有效提高了Pt催化剂的电催化活性。
图3是本发明制备的导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO与Pt/rGO的一氧化碳（CO）溶出循环伏安曲线，由图3可看出， Pt/(PPy)3PMo12O40/rGO的CO溶出曲线起始平台电位0.55V小于Pt/rGO的0.63V，说明Pt/(PPy)3PMo12O40/rGO比Pt/rGO具有更好的抗CO中毒性能，证明修饰剂导电聚合物多金属氧酸盐(PPy)3PMo12O40可改善Pt催化剂的抗CO中毒性能。
图4是本发明制备的导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO与Pt/rGO的电化学阻抗图，由图4可看出， Pt/(PPy)3PMo12O40/rGO的电荷转移电阻为2.7Ω，远小于Pt/rGO的7.9Ω，说明Pt/(PPy)3PMo12O40/rGO比Pt/rGO具有更好的导电性，证明修饰剂导电聚合物多金属氧酸盐(PPy)3PMo12O40可改善催化剂的导电性。
具体实施方式
实施例1
将0.7mL吡咯加入玛瑙研钵中冷冻1 h，加入研细的过硫酸铵1.5974g，研磨5 min，再加入研细的钼磷酸(H3PMo12O40·nH2O) 4.2000 g，混合研磨2 h，得到干爽的黑色粉末，将其放置48 h，用水、乙醇和乙醚洗涤得到成分为聚吡咯钼磷酸盐（(PPy)3PMo12O40）的导电聚合物多金属氧酸盐。称取0.02 g (PPy)3PMo12O40，加入1 mL N，N-二甲基甲酰胺溶解，加入25 mL乙二醇，超声5 min混合均匀，再加入0.04 g氧化石墨，超声分散30min，然后依次加入1 mL0.05 mol•L-1的氯铂酸（H2PtCl6）乙二醇溶液和0.4 mL 0.4 mol•L-1的氢氧化钾水溶液，磁力搅拌3 h，使其充分混合， 160 ℃反应3 h后自然冷却至室温，继续搅拌12 h，再用高纯水和丙酮洗涤，60 ℃真空干燥12 h，制得导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO。
Claims (2)
1.一种导电聚合物多金属氧酸盐复合铂催化剂的制备方法，其特征在于按下列步骤进行：0.7mL吡咯置于玛瑙研钵中冷冻1 h后加入研细的过硫酸铵1.5974g研磨5 min，再加入研细的钼磷酸(H3PMo12O40·nH2O) 4.2000 g，混合研磨2 h，得到干爽的黑色粉末，将其放置反应48 h，用水、乙醇和乙醚洗涤得到成分为聚吡咯钼磷酸盐（(PPy)3PMo12O40）的导电聚合物多金属氧酸盐，取其0.02 g置于圆底烧瓶中，加入1 mL N，N-二甲基甲酰胺（DMF）溶解，加入25 mL乙二醇，超声5min混合均匀后再加入0.04 g氧化石墨（GO），超声分散30min，然后依次加入1 mL 0.05 mol•L-1的氯铂酸（H2PtCl6•6H2O）乙二醇溶液和0.4 mL 0.4 mol•L-1的KOH水溶液，磁力搅拌3 h，使其充分混合，160 ℃反应3 h之后自然冷却至室温，继续搅拌12h，用高纯水和丙酮充分洗涤，60 ℃真空干燥12 h，制得导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO。
2.根据权利要求1所述的制备方法，所得的导电聚合物多金属氧酸盐复合铂催化剂Pt/(PPy)3PMo12O40/rGO具有良好的抗一氧化碳中毒性能和甲醇氧化电催化活性。
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