无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2011, Vol. 43 ›› Issue (4): 36-.

• 论文 • 上一篇    下一篇

温和条件下钴酸镍的水热合成

方军1,黄爱红2   

  1. 1.中国广州分析测试中心广东省分析测试技术公共实验室,广东广州 510070;2.中山大学化学与化工学院
  • 发布日期:2011-04-19

Hydrothermal synthesis of nickel cobaltate under milder condition

Fang Jun1,Huang Aihong2   

  1. 1.Guangdong Provincial Public Laboratory of Analysis and Testing Technology,China National Analytical Center,Guangzhou,Guangzhou 510070,China;2.School of Chemistry and Chemical Engineering,Sun Yat-Sen University
  • Published:2011-04-19

摘要: 利用镍、钴的醋酸盐为原料在温和条件下成功地用水热法合成了纯的尖晶石型钴酸镍。用XRD、SEM、TEM、IR对产物进行了表征,并对体系的酸碱性、矿化剂、原料配比、反应温度和反应时间等影响因素进行了研究。矿化剂氨水浓度大于4 mol/L或小于1.5 mol/L,钴、镍的醋酸盐物质的量比大于7∶3或小于2∶1,水热合成温度小于220 ℃,合成时间小于72 h均无法得到纯的钴酸镍。当钴、镍的醋酸盐物质的量比控制在7∶3,加入2.5 mol/L氨水,在220 ℃水热反应72 h可以得到纯的纳米级钴酸镍,并用醋酸洗去少量残存的氧化镍杂质。

关键词: 水热合成, 钴酸镍, 尖晶石

Abstract: Pure spinel-type nickel cobaltate (NiCo2O4) was sucessfully prepared by hydrothermal synthesis method under milder reaction conditions with nickel acetate and cobalt acetate as raw materials.Product was characterized by XRD,SEM,TEM,and IR.Influencing factors,such as acid-base property,mineralizers,raw material mix ratio,time,and temperature,of the reaction system were invesitgated.When the concentration of mineralizer NH3•H2O was more than 4 mol/L or less than 1.5 mol/L,amount-of-substance ratio of cobalt acetate to nickel acetate was higher than 7∶3 or lower than 2∶1,hydrothermal synthesis temperature was below 220 ℃ and synthesis time was less than 72 h,no pure NiCo2O4 will be obtained.On the other hand,under the conditions that amount-of-substance ratio of Co to Ni was 7∶3,c(NH3•H2O)=2.5 mol/L,hydrothermal reacting at 220 ℃ for 72 h,pure NiCo2O4 nano6-particles could be obtained after using acetic acid to wash a small amount of nickel oxide impurity.

Key words: hydrothermal synthesis, nickel cobaltate, spinel

中图分类号: