CN104098146B - 一种八面体状Co3O4纳米材料的熔融盐制备法及应用 - Google Patents

一种八面体状Co3O4纳米材料的熔融盐制备法及应用 Download PDF

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CN104098146B
CN104098146B CN201410333931.3A CN201410333931A CN104098146B CN 104098146 B CN104098146 B CN 104098146B CN 201410333931 A CN201410333931 A CN 201410333931A CN 104098146 B CN104098146 B CN 104098146B
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CN104098146A (zh
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邓积光
何胜男
戴洪兴
谢少华
杨黄根
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Beijing University of Technology
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Abstract

一种八面体状Co3O4纳米材料的熔融盐制备法及应用,属于纳米材料制备技术领域。首先将按比例称量的NaNO3、NaF和CoCl2混合均匀后,转移至马弗炉内,以1℃/min的速率从室温升至350-500℃,保温1-5h,自然冷却至室温,经溶解、抽滤、洗涤、干燥后,即得八面体状Co3O4纳米材料。本发明具有原料廉价易得,制备过程简单,产物形貌可控和催化性能好等优势。

Description

一种八面体状Co3O4纳米材料的熔融盐制备法及应用
技术领域
本发明涉及一种制备八面体状Co3O4纳米材料的熔融盐法,具体的说涉及以NaNO3和NaF为熔融盐体系制备八面体状Co3O4纳米材料的熔融盐法,属于纳米材料制备技术领域。
背景技术
工业废气【如挥发性有机物(VOC)等】污染大气环境,危害人身健康。催化燃烧法是目前最常用的去除VOC的技术之一。在催化剂作用下,VOC可在较低温度(<500℃)下完全氧化,去除率通常高于95%。催化燃烧法的关键是催化剂的选择。目前用于催化VOC燃烧的催化剂主要包括负载型贵金属催化剂和过渡金属氧化物催化剂。跟负载型贵金属催化剂相比,过渡金属氧化物催化剂来源广泛,价格低廉,因而倍受关注。熔融盐法是近年来发展起来的制备纳米材料的新方法。例如Ji等(B.T.Ji,etal.,CrystEngComm,2010,12:3229-3234)以NaNO3/NaF为熔融盐体系,制备得到对CO氧化反应具有较高催化活性的α-Mn2O3纳米线催化剂。Jiang等(Z.Y.Jiang,etal.,J.Phys.Chem.B,2005,109:23269-23273)采用熔融盐法,在LiCl熔融盐体系中获得ZnO纳米线。Wang等(W.Z.Wang,etal.,J.Cryst.Growth,2009,311:4275-4280)采用熔融盐法,在NaCl熔融盐体系中制备出CoO纳米线。Liu等(B.Liu,etal.,J.Am.Chem.Soc,2013,135:9995-9998)采用熔融盐法,在NaCl/Na2HPO4熔融盐体系中制备出TiO2纳米线。值得指出的是,目前尚无采用熔融盐法,在NaNO3和NaF熔融盐体系中制备出八面体状Co3O4纳米材料的文献报道。
发明内容
本发明的目的在于提供一种制备八面体状Co3O4纳米材料的熔融盐制备法。
一种制备八面体状Co3O4纳米材料的熔融盐制备法,其特征在于,将NaNO3、NaF和CoCl2混合球磨均匀后,转移至马弗炉内,以1℃/min的速率从室温升至350-500℃,并在此温度下保温1-5h,自然冷却至室温,经溶解、抽滤、洗涤、干燥后,即得八面体状Co3O4纳米材料。优选NaNO3与NaF的质量比为49:1,(NaNO3+NaF)与CoCl2的质量比为3:1。
本发明的八面体状Co3O4纳米材料在甲苯完全氧化反应中的应用。
本发明具有原料廉价易得,制备过程简单,产物粒子形貌和晶体结构可控,以及产量高等优点。所得八面体状Co3O4纳米材料在电极材料、催化剂、超导材料、传感器、合成气生产、环境监测等方面具有潜在的良好的应用前景。利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)等技术分别表征了样品的晶相结构和粒子形貌。
附图说明
图1为所得八面体状Co3O4纳米材料的XRD谱图,其中曲线(a)、(b)分别为实施例1、实施例2在350℃和500℃条件下焙烧后的XRD谱图。
图2为所得八面体状Co3O4纳米材料的SEM照片,其中(a)、(b)分别为实施例1、实施例2在350℃和500℃条件下焙烧后的SEM照片。
图3为所得八面体状Co3O4纳米材料对甲苯完全氧化反应的催化活性,其中曲线(a)、(b)分别为实施例1、实施例2催化剂在甲苯浓度为1000ppm、甲苯与氧气摩尔比为1/400和空速为20000mL/(gh)条件下的甲苯氧化活性曲线。
具体实施方式
为进一步了解本发明,下面以实施例作详细说明,并给出附图描述本发明得到的八面体状Co3O4纳米材料,但本发明并不限于以下实施例。
实施例1:将29.4gNaNO3、0.6gNaF与10gCoCl2混合球磨15min,混合均匀后转移至马弗炉中,以1℃/min的升温速率从室温升至350℃,保温1h,随后自然冷却至室温,经溶解、抽滤、洗涤、干燥后,即可得到八面体状的Co3O4纳米材料。
实施例2:将29.4gNaNO3、0.6gNaF与10gCoCl2混合球磨15min,混合均匀后转移至马弗炉中,以1℃/min的升温速率从室温升至500℃,保温5h,随后自然冷却至室温,经溶解、抽滤、洗涤、干燥后,即可得到八面体状的Co3O4纳米材料。
本发明制备方法新颖,原料廉价,制备过程简单,产物粒子形貌可控且产量较高。所得八面体状Co3O4纳米材料在催化化学领域具有潜在的应用价值。

Claims (2)

1.一种制备八面体状Co3O4纳米材料的熔融盐制备方法,其特征在于,将NaNO3、NaF和CoCl2混合球磨均匀后,转移至马弗炉内,以1℃/min的速率从室温升至350-500℃,并在此温度下保温1-5h,自然冷却至室温,经溶解、抽滤、洗涤、干燥后,即得八面体状Co3O4纳米材料。
2.按照权利要求1的一种制备八面体状Co3O4纳米材料的熔融盐制备方法,其特征在于,NaNO3与NaF的质量比为49:1,(NaNO3+NaF)与CoCl2的质量比为3:1。
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CN105271440B (zh) * 2015-09-29 2017-03-08 曲阜师范大学 一种纳米四氧化三钴的制备方法
CN111172743B (zh) * 2020-01-16 2021-10-19 浙江大学 一种低温快速制备复合金属氧化物纳米薄膜材料的方法
CN114522690B (zh) * 2022-01-15 2023-03-24 中国科学院地球环境研究所 一种熔融盐法制备的富含氧空位的超薄四氧化三钴纳米片催化剂及制备方法
CN114749180B (zh) * 2022-04-02 2023-04-25 南昌航空大学 一种自生长熔融盐辅助的四氧化三钴催化剂的制备方法及应用
CN116351423B (zh) * 2023-04-04 2024-05-03 河北科技师范学院 Cu-Co3O4催化剂及其制备方法与应用

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US8197707B2 (en) * 2006-09-08 2012-06-12 Signa Chemistry Llc Lithium-porous metal oxide compositions and lithium reagent-porous metal compositions
CN103086441A (zh) * 2013-01-15 2013-05-08 西安交通大学 一种纳米Co3O4八面体粉末的制备方法

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CN102134104A (zh) * 2011-03-29 2011-07-27 长沙拓智金属材料科技有限责任公司 钴盐沉淀微波诱导热解法制备超细八面体四氧化三钴的方法
CN103086441A (zh) * 2013-01-15 2013-05-08 西安交通大学 一种纳米Co3O4八面体粉末的制备方法

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