CN115318294A - 一种低成本自还原法合成的碳载双金属催化剂及其应用 - Google Patents
一种低成本自还原法合成的碳载双金属催化剂及其应用 Download PDFInfo
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Abstract
本发明是一种低成本固相自还原法合成的碳载双金属纳米催化剂及其应用,合成方法为将树叶、秸秆、甘蔗渣、水果皮等生物质炭BC(Biomass Charcoal)材料洗净、烘干并粉碎成粉末;将硝酸盐和生物质粉末完全溶解在去离子水中,并在真空干燥箱中烘干;将干燥后的样品放入管式炉中,在氮气氛围下进行煅烧,利用碳自身的还原性,原位生成双金属碳载纳米催化剂MN/BC(M、N代表两种不同的金属)。双金属催化剂可以应用于各种脱氢、加氢的反应中,提高加氢和脱氢的速率,比如储氢材料的吸脱氢反应、糠醛和乙酰丙酸的加氢反应等。该制备方法简单、环保、成本低廉,有助于提高各种加氢脱氢反应的进行。本发明所用原料来源丰富,制备方法成熟,操作过程可控,是一种对加氢脱氢反应性能优良的催化剂。
Description
技术领域
本发明属于催化材料领域,具体说涉及一种用于储氢材料的加氢脱氢反应、糠醛和乙酰丙酸的加氢反应的低成本碳载双金属纳米催化剂的制备方法以及对加氢脱氢性能的改善。
背景技术
对于很多的化学反应过程,添加催化剂是提高反应效率最简单高效的策略。负载型催化剂是一类将活性相负载到载体上的催化剂,合适的载体一般具备一定的比表面积和合适的孔道结构以提高活性相金属的分散度,另一方面,载体要有足够的机械强度以保护催化剂在反应时不会被破坏。碳材料作为金属催化剂载体是非常常见的选择,例如活性碳,石墨烯,碳纳米管等。但是无论是商业化的碳材料还是实验室合成的碳材料都具有非常昂贵的价格。这无疑也会增加化学反应的成本。生物质炭材料是由富含碳的生物质在无氧或缺氧条件下经热化学转化生成的一种具有富含碳素的多孔固体颗粒物质,比如常见的秸秆、树叶,柚子皮、甘蔗渣、废旧棉布等。这些物质都是废弃物的回收再利用,成本非常低。众所周知,双金属催化剂由于不同金属间的协同作用而具有更加优良的催化效果。专利CN201610538989.0以及CN202011462072.X提到了FeNi以及NiCu双金属催化剂的合成,但是其合成方法较为复杂,这也进一步的增加了碳载催化剂的合成成本和难度。
发明内容
为了解决上述问题,本发明提供了一种低成本的固相自还原法合成的碳载双金属纳米催化剂,并应用于储氢材料的吸脱氢反应、糠醛和乙酰丙酸的加氢反应等。该方法制备的催化剂价格低廉,操作可控,对加氢脱氢速率起到很好的改善作用。
为了达到上述目的,本发明是通过以下技术方案实现的:
一种低成本碳载双金属纳米催化剂的合成方法,包括如下步骤:
(1)将生物质炭(BC)材料清洗干净,在80℃的真空干燥箱中烘干,并用粉碎机打成粉末。生物质碳材料包括秸秆、甘蔗渣、水果皮、稻壳、废旧棉布等。
(2)将两种不同的硝酸盐与步骤1中的粉末依次加入去离子水中,在磁力搅拌机上搅拌12h。硝酸盐是硝酸镍、硝酸铁、硝酸钴、硝酸铜中的任意两种。
其中两种硝酸盐的摩尔比为1:3-3:1,硝酸盐总质量和生物质粉末的质量比为1:2-4:1。固体物质和去离子水的质量比为1:10-1:15。
(3)将得到的糊状的混合物放入真空干燥箱中80℃干燥24h。
(4)将干燥后的样品放入管式炉中,在氮气氛围下进行煅烧。管式炉从室温以4℃/min的升温速率升温到400℃-750℃。待冷却后制备成功MN/BC(M、N 代表两种不同的金属)纳米催化剂。MN/BC纳米催化剂粒径约4-40nm。
将本发明的MN/BC双金属碳载纳米催化剂应用于MgH2、LiBH4、Mg2Ni储氢材料的加氢脱氢反应、糠醛和乙酰丙酸的加氢反应等。可以大幅改善脱氢加氢速率,加快反应进程。
本发明的有益效果是:
(1)生物质来源丰富,与石墨烯、碳纳米管等碳载体相比,具有绝对的价格优势。
(2)本发明的MN/BC双金属碳载纳米催化剂的制备工艺简单,操作过程可控,能够利用生物质炭一步还原出双金属纳米催化剂,无需添加其他的还原剂。
(3)用到的磁力搅拌器、管式炉等都是市场上的成熟产品,不需要特定设备,MN/BC双金属碳载纳米催化剂作为低廉的催化剂不会增加化学反应的成本;
(4)制备的MN/BC双金属碳载纳米催化剂是粒径只有4-40nm,具有非常优越的加氢脱氢性能。
附图说明
图1是本发明Ni3Fe/BC纳米催化剂的XRD图。
图2是本发明Ni3Fe/BC纳米催化剂的TEM图。
图3是MgH2+10wt%Ni3Fe/BC与MgH2升温脱氢曲线对比图。
图4是MgH2+10wt%Ni3Fe/BC与MgH2升温吸氢曲线对比图。
图5是不同催化剂对糠醛加氢制备糠醇的影响。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细地说明。
本发明是一种低成本碳载双金属纳米催化剂的合成方法,选用食用柚子的皮作为生物质来源,首先将柚子皮用去离子水洗干净之后切成小块,在真空干燥箱中80℃干燥24h,最后用粉碎机粉碎成粉末。取20mL去离子水,依次加入1.13 g Ni(NO3)2·6H2O,0.52gFe(NO3)3·9H2O,在磁力搅拌机上搅拌并完全溶解,然后加入2g柚子皮粉,并继续搅拌12h。最后将糊状的混合物放入真空干燥箱中80℃干燥24h。将干燥后的样品放入管式炉中,在氮气氛围下进行煅烧。管式炉以 2℃/min的升温速率升至750℃,保温3h。待冷却后制备成功Ni3Fe/BC纳米催化剂。制得的Ni3Fe/BC纳米催化剂的XRD图和TEM图如图1-2所示。
实施例1
制备的Ni3Fe/BC纳米催化剂与储氢材料掺杂,测试储氢性能。
本实施例以MgH2为储氢材料,取10wt%Ni3Fe/BC纳米催化剂与90wt% MgH2装入球磨罐,球磨罐中充有0.1MPa Ar,在行星球磨机中以450r/min球磨 5h。对储氢材料进行脱氢性能测试,以2℃/min的升温速率从室温升高到450℃,保温10min,测取升温过程中样品的放氢量,绘制升温脱氢曲线如图3所示, MgH2+10wt%Ni3Fe/BC材料在184.5℃就开始脱氢,到290℃就完成了全部脱氢,而纯MgH2要到350℃才开始脱氢,掺杂Ni3Fe/BC纳米粉末后显著改善了MgH2的脱氢性能。
对脱氢后的储氢材料进行加氢测试,测试氢气压力为3MPa,以1℃/min的升温速率从室温升高到400℃,保温10min,测取升温过程中样品的吸氢量,绘制升温加氢曲线如图4所示。MgH2+10wt%Ni3Fe/BC材料在30℃就可以开始加氢,在200℃可以吸收6wt%H2,而相同条件下MgH2仅吸收1wt%的H2,掺杂 Ni3Fe/BC纳米催化剂后吸氢温度显著降低,可以在较低温度实现吸氢。
实施例2
制备的Ni3Fe/BC纳米催化剂测试糠醛的加氢反应。
向反应釜中加入1.2g糠醛、30g异丙醇以及0.2g Ni3Fe/BC纳米催化剂,将反应釜密封,用H2置换5次以除去釜内空气,然后充H2至所需压力,对装置的气密性进行检查确认装置不漏气后。反应温度为170℃,压力2MPa,确认无误后开启反应釜。反应结束后,待反应釜冷却至室温,取反应液用于分析。为了便于说明,采用了BC和Ni/BC催化剂作为比较对象。测试结果如图5所示。 Ni3Fe/BC纳米催化剂作用下,糠醛的转化率为99.4%,而且具有较好的糠醇选择性。
Claims (8)
1.一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述制备方法包括如下步骤:
步骤1:将生物质炭(BC)材料清洗干净,在80℃的真空干燥箱中烘干,并用粉碎机打成粉末。
步骤2:将两种不同的硝酸盐与步骤1中的粉末依次加入去离子水中,在磁力搅拌机上搅拌12h。
步骤3:将得到的糊状的混合物放入真空干燥箱中80℃干燥24h。
步骤4:将干燥后的样品放入管式炉中,在氮气氛围下进行煅烧。待冷却后制备成功MN/BC(M、N代表两种不同的金属)纳米催化剂。
2.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤1中生物质碳材料包括秸秆、甘蔗渣、水果皮、稻壳、废旧棉布等。
3.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤2中硝酸盐是硝酸镍、硝酸铁、硝酸钴、硝酸铜中的任意两种。
4.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤2中两种硝酸盐的摩尔比为1:3-3:1,硝酸盐总质量和生物质粉末的质量比为1:2-4:1。
5.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤2中固体物质和去离子水的质量比为1:10-1:15。
6.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤4中管式炉从室温以4℃/min的升温速率升温到400℃-750℃。
7.根据权利要求1所述的一种低成本碳载双金属纳米催化剂的合成方法,其特征在于:所述步骤4中的MN/BC纳米催化剂粒径约4-40nm。
8.一种如权利要求1所述MN/BC双金属碳载纳米催化剂可以应用于MgH2、LiBH4、Mg2Ni储氢材料的加氢脱氢反应、糠醛和乙酰丙酸的加氢反应等。
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