改性碳纳米管负载铂—钌催化剂的可控制备及加氢性能
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摘要
碳纳米管(CNT)具有明显不同于传统催化剂载体材料的特性,其作为催化剂载体在多种催化反应以及燃料电池等领域显示了其独特的催化性能,而受到学术和工业界的广泛关注。因此,CNT表面官能团修饰也成为研究的热点之一,但有关表面官能团对CNT负载金属纳米颗粒及其催化性能的影响的文献报道却很少。针对这一问题,本论文发展了混酸氧化-热处理、HNO3气相氧化以及NH3处理方法进行CNT表面官能团化,从而实现了CNT表面官能团种类及数量的可控；并发明了室温下无表面活性剂和修饰剂的贵金属胶体合成方法,探讨了胶体的可能形成机理；通过多醇胶体方法制备CNT负载Pt和Ru催化剂,研究其在1,5-环辛二烯(1,5-COD)和苯乙炔(PA)选择加氢反应中的催化性能。主要结果如下：
采用HNO3-H2SO4混酸处理CNT可以在CNT表面形成丰富的含氧官能团。在惰性气氛下,通过程序升温热处理可以选择性地控制表面官能团的数量和种类。采用乙二醇还原法制备了改性CNT负载Pt催化剂,发现金属Pt的分散度和抗烧结能力与载体表面含氧官能团的种类及数量有关,但含氧官能团对Pt的担载量却无明显影响。苯乙炔(PA)加氢结果显示CNT表面官能团种类不影响PA选择加氢反应速率,且苯乙烯(ST)的选择性不受Pt粒径的影响。PA选择加氢TOF随Pt粒径的增加而增加,表明PA选择加氢反应是结构敏感反应。
HNO3气相氧化可在CNT表面生成含氧官能团。气相氧化过程中碳刻蚀导致CNT的比表面积增加,同时氧含量和表面酸性也随着氧化时间的增加而增加,随着处理温度的增加而减小。而高温NH3处理气相氧化后的CNT可以引入含氮官能团,氮含量与氧化CNT中氧含量成正比,高浓度NH3降低了CNT的比表面积。氧官能团或氮官能团的引入均降低了CNT的热稳定性。
CNT负载Pt催化剂用于1,5-COD气相选择加氢反应,结果表明在1-6%H2浓度范围内,H2的反应级数为1/2,而1,5-COD的反应级数为0。1,5-COD选择加氢的TOF随粒径的增加而增加,而COE加氢的TOF和反应物反应级数均不受金属Pt粒径的影响。NH3处理氧化CNT生成的嘧啶类官能团增强了金属Pt纳米颗粒与载体CNT的相互作用,使Pt均匀地分散在CNT表面。与Pt/oCNTs催化剂相比,Pt/NCNTs在1,5-COD加氢反应表现出较高的催化活性及稳定性。
采用乙二醇还原方法,使用相同的金属前体,选择性地制备出具有不同Pt-Ru结构的双金属(如核-壳,合金,和简单物理混合结构)纳米颗粒。制备的Pt, Ru, Pt-Ru合金，Ru@Pt和Pt@Ru核-壳纳米颗粒的粒径在1.5到3.0纳米之间,可以均匀地分散在CNT表面。CNT负载Pt@Ru和Ru@Pt核壳纳米催化剂在PA选择加氢中显示出不同与具有相同金属组成的Pt-Ru合金和简单的物理混合催化剂的加氢性能。
在室温下,在老化的H2PtCl6乙二醇溶液中引入醋酸钠控制合成了Pt溶胶,并通过调整醋酸钠的浓度从2×10-3-2×10-1mol/l可以调控Pt纳米颗粒的粒径在2.4-4.2nm之间。研究认为室温下乙二醇还原法制备Pt溶胶的反应机理如下：老化的过程中生成易还原的配合物H2PtCl4(EG)n;然后此配合物在醋酸钠存在下使Pt离子还原为Pt金属纳米颗粒,而乙二醇氧化生成羟基乙醛；生成的羟基乙醛不稳定易被进一步氧化生成羟基乙酸；醋酸钠促进了配合物H2PtCl4(EG)n的还原,并稳定了生成的Pt胶体。
CNT is a novel catalytic material with unique structure and properties and has drawn much attention as a potential catalytic material from a viewpoint of both fundamental research and industrial uses. It has been demonstrated that the use of CNTs as catalyst support can improve activity and selectivity in hydrogenation and electrocatalysis. Meanwhile, the oxygen-containing surface groups on CNTs also have received more and more attention, but only a few studies have been directed at elucidating the influence of the surface oxygen groups on the catalytic behavior of the CNTs-supported catalysts. In terms of current issues, we have developed oxidative treatments of CNTs with HNO3-H2SO4followed by thermal treatments to control the type of the surface oxygen groups or HNO3vapor treatment was applied for the oxygen and nitrogen functionalization of CNTs. Pt colloids have been synthesized at room temperature through simply introducing acetate to the aged ethylene glycol (EG) solution of H2PtCl6and the possible formation process was also discussed. Pt/CNTs was achieved through chemical reduction of H2PtCl6·6H2O by EG in the presence of NaOH. Selective hydrogenation of PA and1,5-COD were used as probe reaction to evaluate their catalytic performances. The main results are as follows.
CNTs with different surface groups were achieved by oxidative treatments with HNO3-H2SO4followed by thermal treatments. The type and amount of surface oxygen functional groups on the CNTs can be tuned by thermal treatments at different temperatures in an inert atmosphere. Deposition of Pt particles onto CNTs was achieved through chemical reduction of H2PtCl6·6H2O by EG in the presence of NaOH. Both dispersion and sintering resistance of Pt nanoparticles were found to be a function of amount of oxygen surface groups on the carbon nanotubes, however, the amount of oxygen surface groups apparently did not affect the Pt loading on the CNTs. For the hydrogenation of PA, the TOF increased linearly when the Pt particle size increases, whereas the selectivity to ST did not depend on particle size.
Gas-phase methods were applied for the oxygen and nitrogen functionalization of CNTs. The oxygen functionalization was performed by HNO3vapor treatment at temperatures from200℃to250℃for12h up to120h. The oxygen-functionalized CNTs were used as starting material for nitrogen functionalization through thermal treatment under NH3. The BET surface area increased after the treatment in HNO3vapor, which also caused the weight loss due to carbon corrosion. The oxygen content and the surface acidity increased with increasing treatment time, but decreased with increasing temperature. As to nitrogen functionalization, the amount of nitrogen was correlated with the oxygen amount in the starting CNTs. A higher NH3concentration resulted in lower BET surface area due to carbon corrosion. The incorporation of both oxygen and nitrogen lowered the thermostability of CNTs.
The prepared Pt/CNTs catalysts were evaluated for their performance as catalysts in the hydrogenation of1,5-COD. The reaction is1/2order with respect to H2in the investigated range of1%to6%, and zero order to COD. In the hydrogenation of1,5-COD, it was observed that TOF increases linearly when the Pt particle size increased. However, the TOF of COE remained constant independent of the Pt particle size. Formation of the nitrogen-containing sites with a pyridine-like state should enhance the adhesion between platinum particles and support to stabilizing platinum in a more dispersed state. Pt/NCNTs catalyst due to the higher dispersion of metal displayed higher activity and stability than Pt/oCNTs.
Through the use of the same precursors and protocols, Pt-Ru bimetallic nanoparticles with different structures (i.e., core-shell, alloy, and mixtures of monometallic NP) can be prepared selectively. The prepared Pt, Ru, Pt-Ru alloy, Ru@Pt and Pt@Ru nanoparticles fell in the range of1.5-3.0nm in diameter, and were uniformly dispersed on the CNTs. The Pt@Ru/CNTs and Ru@Pt/CNTs core-shell catalysts showed different catalytic properties in selective hydrogenation of phenylacetylene from the Pt-Ru alloy, and the mixed monometallic samples with the correspondingly identical composition.
Pt colloids have been synthesized at room temperature through simply introducing acetate to the aged EG solution of H2PtCl6without any other capping agents or surfactants. The amount of acetate added to the reaction solution played a key role in producing Pt colloids and adjusting the size of the Pt nanoparticles. The Pt particle sizes were controlled in the range from2.4to4.2nm by changing the concentration of acetate from2×10-3to3.2×10-1M. The possible formation mechanism is the formation of H2PtCl4(EG)n in the process of aging. During reducing Pt ions by EG, CH3COONa plays the role of catalyst and stabilizing agent. For this reaction pathway to take place, the-OH groups of ethylene glycol interact with Pt-ion sites, resulting in the oxidation of the alcohol groups to aldehydes. These aldehydes are not very stable and can be easily oxidized to glycolic.
采用HNO3-H2SO4混酸处理CNT可以在CNT表面形成丰富的含氧官能团。在惰性气氛下,通过程序升温热处理可以选择性地控制表面官能团的数量和种类。采用乙二醇还原法制备了改性CNT负载Pt催化剂,发现金属Pt的分散度和抗烧结能力与载体表面含氧官能团的种类及数量有关,但含氧官能团对Pt的担载量却无明显影响。苯乙炔(PA)加氢结果显示CNT表面官能团种类不影响PA选择加氢反应速率,且苯乙烯(ST)的选择性不受Pt粒径的影响。PA选择加氢TOF随Pt粒径的增加而增加,表明PA选择加氢反应是结构敏感反应。
HNO3气相氧化可在CNT表面生成含氧官能团。气相氧化过程中碳刻蚀导致CNT的比表面积增加,同时氧含量和表面酸性也随着氧化时间的增加而增加,随着处理温度的增加而减小。而高温NH3处理气相氧化后的CNT可以引入含氮官能团,氮含量与氧化CNT中氧含量成正比,高浓度NH3降低了CNT的比表面积。氧官能团或氮官能团的引入均降低了CNT的热稳定性。
CNT负载Pt催化剂用于1,5-COD气相选择加氢反应,结果表明在1-6%H2浓度范围内,H2的反应级数为1/2,而1,5-COD的反应级数为0。1,5-COD选择加氢的TOF随粒径的增加而增加,而COE加氢的TOF和反应物反应级数均不受金属Pt粒径的影响。NH3处理氧化CNT生成的嘧啶类官能团增强了金属Pt纳米颗粒与载体CNT的相互作用,使Pt均匀地分散在CNT表面。与Pt/oCNTs催化剂相比,Pt/NCNTs在1,5-COD加氢反应表现出较高的催化活性及稳定性。
采用乙二醇还原方法,使用相同的金属前体,选择性地制备出具有不同Pt-Ru结构的双金属(如核-壳,合金,和简单物理混合结构)纳米颗粒。制备的Pt, Ru, Pt-Ru合金，Ru@Pt和Pt@Ru核-壳纳米颗粒的粒径在1.5到3.0纳米之间,可以均匀地分散在CNT表面。CNT负载Pt@Ru和Ru@Pt核壳纳米催化剂在PA选择加氢中显示出不同与具有相同金属组成的Pt-Ru合金和简单的物理混合催化剂的加氢性能。
在室温下,在老化的H2PtCl6乙二醇溶液中引入醋酸钠控制合成了Pt溶胶,并通过调整醋酸钠的浓度从2×10-3-2×10-1mol/l可以调控Pt纳米颗粒的粒径在2.4-4.2nm之间。研究认为室温下乙二醇还原法制备Pt溶胶的反应机理如下：老化的过程中生成易还原的配合物H2PtCl4(EG)n;然后此配合物在醋酸钠存在下使Pt离子还原为Pt金属纳米颗粒,而乙二醇氧化生成羟基乙醛；生成的羟基乙醛不稳定易被进一步氧化生成羟基乙酸；醋酸钠促进了配合物H2PtCl4(EG)n的还原,并稳定了生成的Pt胶体。
CNT is a novel catalytic material with unique structure and properties and has drawn much attention as a potential catalytic material from a viewpoint of both fundamental research and industrial uses. It has been demonstrated that the use of CNTs as catalyst support can improve activity and selectivity in hydrogenation and electrocatalysis. Meanwhile, the oxygen-containing surface groups on CNTs also have received more and more attention, but only a few studies have been directed at elucidating the influence of the surface oxygen groups on the catalytic behavior of the CNTs-supported catalysts. In terms of current issues, we have developed oxidative treatments of CNTs with HNO3-H2SO4followed by thermal treatments to control the type of the surface oxygen groups or HNO3vapor treatment was applied for the oxygen and nitrogen functionalization of CNTs. Pt colloids have been synthesized at room temperature through simply introducing acetate to the aged ethylene glycol (EG) solution of H2PtCl6and the possible formation process was also discussed. Pt/CNTs was achieved through chemical reduction of H2PtCl6·6H2O by EG in the presence of NaOH. Selective hydrogenation of PA and1,5-COD were used as probe reaction to evaluate their catalytic performances. The main results are as follows.
CNTs with different surface groups were achieved by oxidative treatments with HNO3-H2SO4followed by thermal treatments. The type and amount of surface oxygen functional groups on the CNTs can be tuned by thermal treatments at different temperatures in an inert atmosphere. Deposition of Pt particles onto CNTs was achieved through chemical reduction of H2PtCl6·6H2O by EG in the presence of NaOH. Both dispersion and sintering resistance of Pt nanoparticles were found to be a function of amount of oxygen surface groups on the carbon nanotubes, however, the amount of oxygen surface groups apparently did not affect the Pt loading on the CNTs. For the hydrogenation of PA, the TOF increased linearly when the Pt particle size increases, whereas the selectivity to ST did not depend on particle size.
Gas-phase methods were applied for the oxygen and nitrogen functionalization of CNTs. The oxygen functionalization was performed by HNO3vapor treatment at temperatures from200℃to250℃for12h up to120h. The oxygen-functionalized CNTs were used as starting material for nitrogen functionalization through thermal treatment under NH3. The BET surface area increased after the treatment in HNO3vapor, which also caused the weight loss due to carbon corrosion. The oxygen content and the surface acidity increased with increasing treatment time, but decreased with increasing temperature. As to nitrogen functionalization, the amount of nitrogen was correlated with the oxygen amount in the starting CNTs. A higher NH3concentration resulted in lower BET surface area due to carbon corrosion. The incorporation of both oxygen and nitrogen lowered the thermostability of CNTs.
The prepared Pt/CNTs catalysts were evaluated for their performance as catalysts in the hydrogenation of1,5-COD. The reaction is1/2order with respect to H2in the investigated range of1%to6%, and zero order to COD. In the hydrogenation of1,5-COD, it was observed that TOF increases linearly when the Pt particle size increased. However, the TOF of COE remained constant independent of the Pt particle size. Formation of the nitrogen-containing sites with a pyridine-like state should enhance the adhesion between platinum particles and support to stabilizing platinum in a more dispersed state. Pt/NCNTs catalyst due to the higher dispersion of metal displayed higher activity and stability than Pt/oCNTs.
Through the use of the same precursors and protocols, Pt-Ru bimetallic nanoparticles with different structures (i.e., core-shell, alloy, and mixtures of monometallic NP) can be prepared selectively. The prepared Pt, Ru, Pt-Ru alloy, Ru@Pt and Pt@Ru nanoparticles fell in the range of1.5-3.0nm in diameter, and were uniformly dispersed on the CNTs. The Pt@Ru/CNTs and Ru@Pt/CNTs core-shell catalysts showed different catalytic properties in selective hydrogenation of phenylacetylene from the Pt-Ru alloy, and the mixed monometallic samples with the correspondingly identical composition.
Pt colloids have been synthesized at room temperature through simply introducing acetate to the aged EG solution of H2PtCl6without any other capping agents or surfactants. The amount of acetate added to the reaction solution played a key role in producing Pt colloids and adjusting the size of the Pt nanoparticles. The Pt particle sizes were controlled in the range from2.4to4.2nm by changing the concentration of acetate from2×10-3to3.2×10-1M. The possible formation mechanism is the formation of H2PtCl4(EG)n in the process of aging. During reducing Pt ions by EG, CH3COONa plays the role of catalyst and stabilizing agent. For this reaction pathway to take place, the-OH groups of ethylene glycol interact with Pt-ion sites, resulting in the oxidation of the alcohol groups to aldehydes. These aldehydes are not very stable and can be easily oxidized to glycolic.
引文
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