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现代化工  2020, Vol. 40 Issue (6): 83-88    DOI: 10.16606/j.cnki.issn0253-4320.2020.06.018
  科研与开发 本期目录 | 过刊浏览 | 高级检索 |
碱式碳酸镍前驱体合成过程调控及其焙烧制球形氧化镍的研究
陈彦广1,2, 于加蒙1,2, 张亚男1,2, 徐瑞晗1,2, 邓冀童1,2, 韩洪晶1,2
1. 东北石油大学化学化工学院, 黑龙江 大庆 163318;
2. 黑龙江省石油与天然气化工省重点实验室, 黑龙江 大庆 163318
Regulation of synthesis process of basic nickel carbonate and study on preparation of spherical nickel oxides through calcination
CHEN Yan-guang1,2, YU Jia-meng1,2, ZHANG Ya-nan1,2, XU Rui-han1,2, DENG Ji-tong1,2, HAN Hong-jing1,2
1. School of Chemistry and Chemical Engineering, Northeast Petroleum University, Daqing 163318, China;
2. Heilongjiang Provincial Key Laboratory of Oil and Gas Chemical Technology, Daqing 163318, China
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摘要 以水热法合成碱式碳酸镍前驱体,通过焙烧制备高比表面积的球形氧化镍,探索了合成过程中碱式碳酸镍晶型、粒径、形貌的调控规律,研究了前驱体热性能及其焙烧机制,并测定了球形氧化镍的孔径和比表面积。结果表明,球形碱式碳酸镍合成的工艺参数为:T=100℃、t=10 h、pH=8、n[Ni(NO32]:n[CO(NH22]=1:2,加入共溶剂有助于调控其形貌和分散程度,在乙醇体积分数为50%的溶液中,合成的球形碱式碳酸镍结构规整,呈均匀的球形结构,粒径为5 μm。热重实验结果表明,碱式碳酸镍500℃分解完全,其优化焙烧参数为:焙烧温度为500℃、焙烧时间为1 h,此时得到的NiO呈立方晶相,为分散均匀的球状,粒径为5 μm,其比表面积和孔径分别为81.92 m2/g和30.18 nm,在孔径保持基本不变的情况下,比普通氧化镍比表面积增大了1倍,孔容提高了2.5倍。
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陈彦广
于加蒙
张亚男
徐瑞晗
邓冀童
韩洪晶
关键词:  水热法  纳米晶  氧化镍    
Abstract: It is an effective way to synthesize morphological adjustable metal oxides from precursors.Basic nickel carbonate precursor is prepared by hydrothermal synthesis.Spherical nickel oxide with high specific surface area is obtained via calcination of basic nickel carbonate.The rules to regulate crystal form,particle size and morphology of basic nickel carbonate are explored.Thermal properties and calcination mechanism of basic nickel carbonate precursor are studied,and the pore size and specific surface area of spherical nickel oxides are measured.Results indicate that the process parameters for the synthesis of spherical basic nickel carbonate are as follows:T=100℃,t=10 h,pH=8,n(Ni(NO3)2):n(CO(NH2)2)=1:2.The addition of co-solvent is helpful to adjust the morphology and dispersion of spherical basic nickel carbonate.In the 20 mL solution with an ethanol volume fraction of 50%,the prepared spherical basic nickel carbonate exhibits uniform in structure with a particle size of 5 μm.Thermogravimetric experiment results show that the prepared basic nickel carbonate decomposes completely at 500℃.Its optimal calcination parameters include T=500℃ and t=1 h,under which the obtained NiO shows a cubic crystalline phase,uniformly dispersed sphere with a particle size of 5 μm,and its specific surface area and pore size are 81.92 m2·g-1 and 30.18 nm.Compared with common nickel oxide,its specific surface area and pore volume increases by 1 times and 2.5 times as its pore size remains basically unchanged.
Key words:  hydrothermal method    nanocrystals    nickel oxides
收稿日期:  2019-08-07      修回日期:  2020-04-10          
ZTFLH:  TQ138.13  
基金资助: 国家自然科学基金(51674089);黑龙江省优秀青年基金(JC2018002);黑龙江省博士后科研发展基金(LBH-Q16037);东北石油大学研究生创新计划项目(JYCX-CX03-2018)
通讯作者:  陈彦广(1979-),男,博士,教授,研究方向为催化材料制备过程调控及能源催化转化利用,通讯联系人,ygchen79310@126.com。    E-mail:  ygchen79310@126.com
引用本文:    
陈彦广, 于加蒙, 张亚男, 徐瑞晗, 邓冀童, 韩洪晶. 碱式碳酸镍前驱体合成过程调控及其焙烧制球形氧化镍的研究[J]. 现代化工, 2020, 40(6): 83-88.
CHEN Yan-guang, YU Jia-meng, ZHANG Ya-nan, XU Rui-han, DENG Ji-tong, HAN Hong-jing. Regulation of synthesis process of basic nickel carbonate and study on preparation of spherical nickel oxides through calcination. Modern Chemical Industry, 2020, 40(6): 83-88.
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https://www.xdhg.com.cn/CN/10.16606/j.cnki.issn0253-4320.2020.06.018  或          https://www.xdhg.com.cn/CN/Y2020/V40/I6/83
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