CN107185524A - 一种三维石墨烯‑贵金属纳米催化剂的制备方法 - Google Patents
一种三维石墨烯‑贵金属纳米催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种三维石墨烯‑贵金属纳米催化剂的制备方法，具体包括以下步骤：氧化石墨烯分散液与贵金属前驱体、一定量的交联剂水热交联，干燥后煅烧，即得到三维石墨烯‑贵金属纳米催化剂。本发明的有益效果是：采用一锅法制备出的三维石墨烯‑贵金属纳米催化剂无需添加还原剂，复合材料结构稳定，贵金属纳米粒子均匀分散在石墨烯的表面，复合材料在电催化、化学催化、能源存储与转换、生物传感等领域就有广阔的应用前景。
Description
技术领域
本发明涉及一种三维石墨烯-贵金属纳米催化剂的制备方法，属于材料合成技术领域。
背景技术
贵金属主要包括金、银、铂族(锇、铱、铂、钌、铑、钯)等金属，其在材料、化学化工等领域具有广泛的应用。贵金属自身大都具有很高的催化活性，可是由于它们存储量十分稀缺，因此价格昂贵。贵金属催化剂的活性受很多因素影响，除了受金属本身的影响，还与其表面积、孔隙率和载体的性质等因素有关，为此要想制备高效催化剂，降低催化剂成本，其中的活性物质就要实现充分微粒化，使比表面积增大。但是贵金属单独实现微粒化不太容易，一方面是因为得到的粒子不稳定；另一方面粒子在制备过程中易长大团聚。目前常用的解决办法就是把催化剂的活性物质充分分散在合适载体表面。
石墨烯因为其优异的电学、光学、力学及热学性能，在材料领域有广泛的应用。石墨烯具有较大的比表面积、良好的化学稳定性以及导电性等优点，理论上是贵金属纳米粒子的优异载体，但由于石墨烯表面能很高，二维的石墨烯片层之间极易团聚，大大降低了其实际性能，将二维石墨烯组装成三维石墨烯是防止石墨烯团聚的一种有效方法。常规的三维石墨烯一般通过冷冻干燥法制备，采用这种方法制备的三维石墨烯机械稳定性较差，遇溶剂后结构会坍塌，因此负载贵金属纳米粒子后对复合材料的性能仍提升有限。
发明内容
针对背景技术中存在的问题，本发明提供一种三维石墨烯-贵金属纳米催化剂的制备方法，通过下述步骤制得：
1、一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于，制备过程包括以下步骤：
a、将氧化石墨烯超声分散于水中，制备一定浓度的氧化石墨烯分散液；然后与贵金属化合物、交联剂混合；在水热反应釜中一定温度下水热反应12h，形成的水凝胶干燥，得到干凝胶；
b、将步骤a得到的干凝胶在氩气下，一定温度下煅烧，得到三维石墨烯-贵金属纳米催化剂。
上述步骤a所述的氧化石墨烯的浓度为1-20mg/mL；
上述步骤a所述的交联剂为三聚氰胺甲醛树脂、苯酚甲醛树脂或尿醛树脂；
上述步骤a所述氧化石墨烯和交联剂的质量比为1:1～1:10；
上述步骤a所述的水热反应的温度为120～180℃；
上述步骤a所述的贵金属化合物为氯铂酸、氯钯酸铵、氯金酸、硝酸银、氯化钌；
上述步骤b所述的煅烧温度为550～850℃加热。
本发明的有益效果是：该法制得的三维石墨烯-贵金属纳米催化剂，结构稳定，具有较大的比表面积，纳米粒子在石墨烯表面分散均匀，克服了常规三维石墨烯-贵金属纳米催化剂易团聚不稳定的缺点。
附图说明
下面结合附图对本发明进一步说明。
图1:本发明制备的纳米铂-三维石墨烯复合材料透射电镜图；
图2:本发明制备的纳米钯-三维石墨烯复合材料透射电镜图；
图3:本发明制备的纳米金-三维石墨烯复合材料透射电镜图；
图4：本发明制备的纳米银-三维石墨烯复合材料透射电镜图；
图5：本发明制备的纳米钌-三维石墨烯复合材料透射电镜图。
具体实施方式
下面结合具体的实施例，进一步详细地描述本发明。应理解，这些实施例只是为了举例说明本发明，而非以任何方式限制本发明的范围。
实施例1：
(1)用改良Hummers法，在500mL容器中依次加入120mL浓硫酸、13.3mL浓磷酸，搅拌，在水浴下慢慢升温至50℃，加入1g石墨粉、6g高锰酸钾，搅拌12h，溶液倒入含10mL过氧化氢溶液的冰块上，搅拌冷却至室温，过滤未反应的固体。离心洗涤至中性，干燥，得氧化石墨烯；
(2)称取0.015g GO，加入15mL二次蒸馏水，超声2min，加入1mL的甲醛和0.35g三聚氰胺，2mL 4mg/mL的氯铂酸水溶液，轻轻搅拌；180℃下水热反应12h。将所得固体在80℃下干燥，得到交联剂支撑的干凝胶；
(3)将干凝胶，在氩气氛下，管式炉先以5℃/min的升温速率升温至300℃，再以10℃/min的升温速率升温至550℃，并保温3h，之后待温度降至室温后去取出产品，得到三维石墨烯-铂纳米催化剂。
实施例2：
(1)氧化石墨烯的制备方法同实施例1。
(2)称取0.15g GO，加入30mL二次蒸馏水，超声2min，加入1mL的甲醛和0.15g苯酚，20mg氯钯酸铵，轻轻搅拌；160℃下水热反应12h。将所得固体在冷冻干燥，得到交联剂支撑的干凝胶；
(3)将干凝胶，在氩气氛下，管式炉先以5℃/min的升温速率升温至300℃，再以10℃/min的升温速率升温至650℃，并保温3h，之后待温度降至室温后去取出产品，得到三维石墨烯-钯纳米催化剂。
实施例3：
(1)氧化石墨烯的制备方法同实施例1。
(2)称取0.15g GO，加入15mL二次蒸馏水，超声2min，加入2mL的甲醛和0.7g尿素，2mL 4mg/mL的氯金酸水溶液，轻轻搅拌；140℃下水热反应12h。将所得固体在80℃下干燥，得到交联剂支撑的干凝胶；
(3)将干凝胶，在氩气氛下，管式炉先以5℃/min的升温速率升温至300℃，再以10℃/min的升温速率升温至750℃，并保温3h，之后待温度降至室温后去取出产品，得到三维石墨烯-金纳米催化剂。
实施例4：
(1)氧化石墨烯的制备方法同实施例1。
(2)称取0.3g GO，加入20mL二次蒸馏水，超声2min，加入1mL的甲醛和0.35g三聚氰胺，40mg硝酸银，轻轻搅拌；120℃下热反应12h。将所得固体在80℃下干燥，得到交联剂支撑的干凝胶；
(3)将交联剂支撑的干凝胶，在氩气氛下，管式炉先以5℃/min的升温速率升温至300℃，再以10℃/min的升温速率升温至850℃，并保温3h，之后待温度降至室温后去取出产品，得到三维石墨烯-银纳米催化剂。
实施例5：
(4)氧化石墨烯的制备方法同实施例1。
(5)称取0.3g GO，加入15mL二次蒸馏水，超声2min，加入1mL的甲醛和0.35g三聚氰胺，40mg氯化钌，轻轻搅拌；120℃下热反应12h。将所得固体在80℃下干燥，得到交联剂支撑的干凝胶；
(6)将交联剂支撑的干凝胶，在氩气氛下，管式炉先以5℃/min的升温速率升温至300℃，再以10℃/min的升温速率升温至550℃，并保温3h，之后待温度降至室温后去取出产品，得到三维石墨烯-钌纳米催化剂。
Claims (7)
1.一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于，制备过程包括以下步骤：
a、将氧化石墨烯超声分散于水中，制备一定浓度的氧化石墨烯分散液；然后与贵金属化合物、交联剂混合；在水热反应釜中一定温度下水热反应12h，形成的水凝胶干燥，得到干凝胶；
b、将步骤a得到的干凝胶在氩气下，一定温度下煅烧，得到三维石墨烯-贵金属纳米催化剂。
2.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤a所述的氧化石墨烯的浓度为1-20mg/mL。
3.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤a所述的交联剂为三聚氰胺甲醛树脂、苯酚甲醛树脂或脲醛树脂。
4.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤a所述氧化石墨烯和交联剂的质量比为1:1～1:10。
5.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤a所述的水热反应的温度为120～180℃。
6.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤a所述的贵金属化合物为氯铂酸、氯钯酸胺、氯金酸、硝酸银、氯化钌。
7.根据权利要求1所述的一种三维石墨烯-贵金属纳米催化剂的制备方法，其特征在于步骤b所述的煅烧温度为550～850℃加热。
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