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 ›› 2021, Vol. 53 ›› Issue (11): 100-106.doi: 10.19964/j.issn.1006-4990.2021-0067

• 环境·健康·安全 • 上一篇    下一篇

氯化胆碱-草酸低共熔溶剂处理含铁尘泥制备纳米氧化铁及动力学研究

曹雪辰(),周东杰,姚海威,居殿春()   

  1. 江苏科技大学张家港校区冶金与材料工程学院,江苏张家港 215600
  • 收稿日期:2021-01-28 出版日期:2021-11-10 发布日期:2021-11-15
  • 作者简介:曹雪辰(1997— ),男,硕士研究生,研究方向为冶金固废资源利用;E-mail: cao19970124@qq.com
  • 基金资助:
    国家自然科学基金面上项目(52072180)

Study on preparation of nanometer iron oxide and its kinetics by CC-OA DES treatment of iron-containing dust

CAO Xuechen(),ZHOU Dongjie,YAO Haiwei,JU Dianchun()   

  1. School of Metallurgy and Materials Engineering,Jiangsu University of Science and Technology,Zhangjiagang 215600,China
  • Received:2021-01-28 Published:2021-11-10 Online:2021-11-15

摘要:

针对钢铁厂含铁尘泥低附加值的问题,以氯化胆碱-二水合草酸(CC-OA)低共熔溶剂(DES)为研究体系,以钢厂含铁粉尘(经水洗处理)为研究对象,提出了运用氯化胆碱-二水合草酸低共熔溶剂处理含铁粉尘固相前驱体热分解法制备纳米氧化铁,并对处理过程中前驱体热分解及纳米氧化铁晶粒生长进行动力学分析。研究表明:处理过程中得到的前驱体为FeC2O4·2H2O,以其热分解第二阶段为热分析动力学的研究目标,根据Ozawa方程法、Kissinger-Akahira-Sunose方程法和Starink方程法3种等转化率法得到的平均反应活化能为220.54 kJ/mol。前驱体焙烧的最佳条件:焙烧温度为673 K、焙烧时间为1 h。根据唯象方程计算出纳米氧化铁的晶粒生长平均激活能为39.06 kJ/mol,并得到了焙烧温度、焙烧时间与粒径的关系,实现特定粒径纳米氧化铁的制备。最佳焙烧条件下得到的纳米氧化铁纯度达99.67%,扫描电镜下观察其颗粒呈现不规则的立方晶体结构,粒径主要分布在10~100 nm。

关键词: 低共熔溶剂, 含铁尘泥, 纳米氧化铁, 动力学

Abstract:

To address the problem of low comprehensive utilization rate of iron-containing dust sludge in steel mills,choline chloride-oxalic acid dihydrate low eutectic solvent(CC-OA DES) was used as the research system,and iron oxide nanoparti-cles were prepared by the thermal decomposition of solid-phase precursors of iron-containing dust treated with CC-OA low eutectic solvent(treated by water washing).The kinetic analysis of the thermal decomposition of the precursor and the growth of iron oxide grains during the treatment was carried out. It was shown that the precursor obtained during the treatment process was FeC2O4·2H2O,and the kinetics of its thermal analysis was targeted at the second stage of thermal decomposition,the average activation energy of 220.54 kJ/mol for the reaction obtained from the three isotropic methods of the Ozawa,Kissinger-Akahira-Sunose and Starink equations.The optimum conditions for precursor roasting: roasting temperature of 673 K and roasting time of 1 h;the average activation energy for grain growth of iron oxide nanoparticles was calculated to be 39.06 kJ/mol according to the only-image equation,and the relationship between roasting temperature,roasting time and grain size was obtained to achieve the preparation of iron oxide nanoparticles of specific grain size;the iron oxide nanoparticles obtained under the optimum roasting conditions had iron oxide with content of 99.67% and were observed an irregular cubic crystal structure under scanning electron microscopy,with particle sizes mainly in the range of 10~100 nm.

Key words: deep eutectic solvent, iron-containing dust, nanometer iron oxide, kinetics

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