CN115555013B - 一种Pt/硅改性氧化铝基催化剂及其制备方法和应用 - Google Patents
一种Pt/硅改性氧化铝基催化剂及其制备方法和应用 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 75
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Abstract
本发明公开一种Pt/硅改性氧化铝基催化剂及其制备方法和应用，属于材料技术领域。该Pt/硅改性氧化铝基催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载。该Pt/硅改性氧化铝基催化剂的制备方法，包括以下步骤：将硅改性氧化铝与水混合分散，之后滴加Pt盐溶液并搅拌得到混合液；将所述混合液干燥得到混合物，将所述混合物在400～500℃下煅烧得到所述Pt/硅改性氧化铝基催化剂。本发明还提出一种上述Pt/硅改性氧化铝基催化剂在柴油尾气催化氧化方面的应用。该催化剂实现了在降低催化剂中贵金属含量的同时有效的提高了催化剂的活性。
Description
技术领域
本发明涉及材料技术领域，具体涉及一种Pt/硅改性氧化铝基催化剂及其制备方法和应用。
背景技术
柴油机的碳氢化合物(HC)和一氧化碳(CO)排放量非常低，但由于一些有害化学物质在较低浓度下存在，它可能具有更高的毒性潜势。1989年，国际癌症研究机构(IARC)通过研究得出结论，柴油机的废气可能对人类致癌。1992年，国际癌症研究机构在得到有关的柴油废气的确凿实验证据后，将其归类为“致癌物”。柴油烟雾已被认为是心血管疾病和哮喘加剧的原因，引起了公众对人类健康和环境危险的认识和关注。
柴油氧化催化剂(DOC)是位于发动机之后的第一个组件，是柴油汽车后处理系统中最重要的组成部分之一。其作用体现三方面：(1)将CO和未燃烧的烃类(HCs)化合物转化为无毒无害的CO2和H2O；(2)辅助下游尾气净化装置，不仅可以在低温下氧化颗粒物中的可溶有机组分以降低潜在的煤烟负荷，同时柴油机废气中的NO被氧化为NO2，具有强的氧化性，可以降低碳烟颗粒物的氧化温度，促进柴油机颗粒捕集器的被动再生；(3)对于氮氧化物减排体系，尤其在运行温度低250℃时，NO优先被氧化，但柴油废气中约90％是NO。因此，DOC将NO氧化为NO2有利于净化尾气中的氮氧化合物。目前，DOC主要采用铂、钯等贵金属作为活性组分，且具有高Pt、Pd负载量，对CO、未燃烧的碳氢化合物和液态烃体现出较高的氧化活性。
许多贵金属已经被证实对CO、HC、NO具有高的催化氧化活性，例如Pd和Pt基催化剂。然而，贵金属存在资源稀缺，价格昂贵等缺点，如何在降低催化剂中贵金属含量的同时有效的提高催化剂的活性仍然是本领域的技术人员亟待解决的技术问题之一。
发明内容
本发明的目的在于克服上述技术不足，提供一种Pt/硅改性氧化铝基催化剂及其制备方法和应用，解决如何在降低催化剂中贵金属含量的同时有效的提高催化剂的活性技术问题。
为达到上述技术目的，本发明的技术方案提供一种Pt/硅改性氧化铝基催化剂，所述催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载。
进一步地，Pt0占所有Pt的比例为50％-55％。
进一步地，硅改性氧化铝载体呈现多孔形貌，Pt/硅改性氧化铝基催化剂平均粒径大小为20-20.5nm。
进一步地，所述Pt与所述硅改性氧化铝的质量比为0.55-0.6:100。
此外，本发明还提出一种Pt/硅改性氧化铝基催化剂的制备方法，包括以下步骤：
将硅改性氧化铝与水混合分散，之后滴加Pt盐溶液并搅拌得到混合液；
将所述混合液干燥得到混合物，将所述混合物在400～500℃下煅烧得到所述Pt/硅改性氧化铝基催化剂。
进一步地，将所述混合液干燥得到混合物包括：先将所述混合液在水浴加热条件下旋蒸，之后微波干燥，之后真空干燥。
进一步地，所述旋蒸的温度为50～70℃；和/或所述真空干燥的时间为10～12小时；和/或，所述搅拌的时间为4-5小时。
进一步地，所述Pt盐溶液为四氨合硝酸铂溶液和氯铂酸溶液中的一种或者两种。
此外，本发明还提出一种Pt/硅改性氧化铝基催化剂，由上述制备方法制备得到。
另外，本发明还提出一种上述Pt/硅改性氧化铝基催化剂在柴油尾气催化氧化方面的应用。
与现有技术相比，本发明的有益效果包括：Pt/硅改性氧化铝基催化剂，所述催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载，只需要Pt与所述硅改性氧化铝的质量比为0.55-0.6:100就具有高催化氧化活性，实现了在降低催化剂中贵金属含量的同时有效的提高了催化剂的活性。
附图说明
图1为实施例1制备的Pt/硅改性氧化铝基催化剂的扫描电镜图；
图2为实施例1中的载体硅改性氧化铝透射电镜图；
图3为实施例1制备的Pt/硅改性氧化铝基催化剂的mapping图；
图4为实施例1制备的Pt/硅改性氧化铝基催化剂的XRD图谱；
图5为实施例1制备的Pt/硅改性氧化铝基催化剂的XPS图谱；
图6为实施例1制备的Pt/硅改性氧化铝基催化剂催化CO、NO、C3H6的转化效率图及稳定性图。
具体实施方式
本具体实施方式提供了一种Pt/硅改性氧化铝基催化剂，所述催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载；其中，Pt0占所有Pt的比例为50％-55％；所述硅改性氧化铝载体呈现多孔形貌，Pt/硅改性氧化铝基催化剂平均粒径大小为20-20.5nm；所述Pt与所述硅改性氧化铝的质量比为0.55-0.6:100。
本具体实施方式还提出一种Pt/硅改性氧化铝基催化剂的制备方法，包括以下步骤：
将硅改性氧化铝与水混合分散，之后滴加Pt盐溶液并搅拌4-5小时得到混合液；
将所述混合液干燥得到混合物，将所述混合物在400～500℃下煅烧4-5小时得到所述Pt/硅改性氧化铝基催化剂；将所述混合液干燥得到混合物包括：先将所述混合液在水浴加热条件下在50～70℃下旋蒸，之后微波干燥30-40s，之后真空干燥10～12小时。
本具体实施方式还提出一种Pt/硅改性氧化铝基催化剂，由上述制备方法制备得到。
本具体实施方式还提出一种上述Pt/硅改性氧化铝基催化剂在柴油尾气催化氧化方面的应用。
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
本实施例提出一种Pt/硅改性氧化铝基催化剂的制备方法，由以下步骤制得：
称取1g硅改性氧化铝粉体并研磨充分，加入20ml水中，超声分散30min以上，称取11mg四氨合硝酸铂，溶于20ml蒸馏水溶液中，待其完全溶解，量取一定量Pt盐溶液缓慢滴加到装有1g硅改性氧化铝粉体的茄形瓶中，使得Pt与载体质量比为0.58％，搅拌4h；
之后在60℃下水浴条件下旋蒸至干，之后在微波炉中干燥30s，然后转移到真空干燥箱中在60℃下干燥12h，最后将干燥所得的粉体在空气下500℃煅烧4h，即得催化剂，命名为Pt/AS5-1，催化剂的产率为99％。催化剂中的Pt以Pt0和Pt2+形式存在，其中Pt0占所有Pt的比例约为52.6％。
本实施例制得的Pt/硅改性氧化铝基催化剂，所述催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载；其中，Pt0占所有Pt的比例为52.6％；所述硅改性氧化铝载体呈现多孔形貌，Pt/硅改性氧化铝基催化剂平均粒径大小为20.4nm；所述Pt与所述硅改性氧化铝的质量比为0.58:100。
针对实施例1所制备的硅改性氧化铝基催化剂，其相关的表征结果如图1～5所示；图1的扫描电镜结果显示催化剂整体呈现块状，图2的投射电镜图可以看出硅改性氧化铝载体呈现多孔形貌，图3可以看出Pt/硅改性氧化铝基催化剂平均粒径大小在20.4nm。图4-5的XRD，Raman及XPS表征结果也进一步证明了Pt/氧化铝基催化剂的成功制备。
实施例1制备的Pt/硅改性氧化铝基催化剂的CO、C3H6、NO的催化氧化活性测试：
在一个直径为5mm管状石英反应器，在大气压力下使用100毫克催化剂，流量340毫升每分钟,气体空速(S.V.)的204000毫升每克每小时。气体由1500ppm CO、900ppm C3H6、600ppm NO、12％O2和N2平衡气组成；催化剂从30℃被加热到550℃；升温为速度2.5℃/min。CO稳定性测试分别选取200℃，220℃进行测试，测试气氛与活性测试条件保持一致，测试时间为72h。
结果如图6所示，Pt/硅改性氧化铝基催化剂催化CO转化率达到50％的温度为205℃，90％的温度为225℃；催化丙烯转化率达到50％的温度为200℃，90％的温度为225℃，具有较大的氧化NO的温度区间，其最高温度下的转化率达到37％，因此实施例1制得的Pt/硅改性氧化铝基催化剂显示良好的催化氧化活性及低温活性。且从图6所示的稳定测试结果看出，在220℃和220℃下进行测试，活性在72h中没有明显的活性下降，表明铂/氧化铝基催化剂显示出了较好的稳定性。
实施例2
本实施例提出一种Pt/硅改性氧化铝基催化剂的制备方法，由以下步骤制得：
称取1g硅改性氧化铝粉体并研磨充分，加入20ml水中，超声分散30min以上，称取11mg四氨合硝酸铂，溶于20ml蒸馏水溶液中，待其完全溶解，量取一定量Pt盐溶液缓慢滴加到装有1g硅改性氧化铝粉体的茄形瓶中，使得Pt与载体质量比为0.58％，搅拌4h；
之后在50℃下水浴条件下旋蒸至干，之后在微波炉中干燥30s，然后转移到真空干燥箱中在60℃下干燥10h，最后将干燥所得的粉体在空气下400℃煅烧5h，即得催化剂，催化剂的产率为98.7％。
实施例3
本实施例提出一种Pt/硅改性氧化铝基催化剂的制备方法，由以下步骤制得：
称取1g硅改性氧化铝粉体并研磨充分，加入20ml水中，超声分散30min以上，称取11.6mg氯铂酸，溶于20ml蒸馏水溶液中，待其完全溶解，量取一定量Pt盐溶液缓慢滴加到装有1g硅改性氧化铝粉体的茄形瓶中，搅拌5h；
之后在55℃下水浴条件下旋蒸至干，之后在微波炉中干燥30s，然后转移到真空干燥箱中在60℃下干燥11h，最后将干燥所得的粉体在空气下450℃煅烧5h，即得催化剂，催化剂的产率为98.3％。
本发明通过超声分散、微波辅助法结合浸渍法成功在硅改性氧化铝表面负载高分散Pt颗粒，所制备的催化剂对柴油尾气具有低温催化氧化活性，而且不会因为长时间的高温测试而造成稳定性的下降，提高了催化剂的经济效益及催化剂的热稳定性。
以上所述本发明的具体实施方式，并不构成对本发明保护范围的限定。任何根据本发明的技术构思所做出的各种其他相应的改变与变形，均应包含在本发明权利要求的保护范围内。
Claims (5)
1.一种Pt/硅改性氧化铝基催化剂的制备方法，其特征在于，包括以下步骤：
将硅改性氧化铝与水混合，超声分散，之后滴加Pt盐溶液并搅拌得到混合液；
将所述混合液干燥得到混合物，将所述混合物在400～500℃下煅烧得到所述Pt/硅改性氧化铝基催化剂；将所述混合液干燥得到混合物包括：先将所述混合液在水浴加热条件下旋蒸，之后微波干燥30-40s，之后真空干燥；Pt/硅改性氧化铝基催化剂中，硅改性氧化铝载体呈现多孔形貌，所述Pt/硅改性氧化铝基催化剂平均粒径大小为20-20.5nm，所述Pt与所述硅改性氧化铝的质量比为0.55-0.6:100；所述旋蒸的温度为50～70℃；所述催化剂以硅改性氧化铝为载体，Pt以Pt0和Pt2+两种形式负载，Pt0占所有Pt的比例为50%-55%。
2.根据权利要求1所述的Pt/硅改性氧化铝基催化剂的制备方法，其特征在于，所述真空干燥的时间为10～12小时。
3.根据权利要求1所述的Pt/硅改性氧化铝基催化剂的制备方法，所述Pt盐溶液为四氨合硝酸铂溶液和氯铂酸溶液中的一种或者两种。
4.一种Pt/硅改性氧化铝基催化剂，其特征在于，由权利要求1-3任一项所述的制备方法制备得到。
5.一种权利要求4所述的Pt/硅改性氧化铝基催化剂在柴油尾气催化氧化方面的应用。
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