利用湿法酸碱调控沉降半焦粉煤渣制备高纯度氧化铁红工艺研究  

Preparation of high purity iron oxide red from settling semi-coke pulverized cinder by wet acid-base regulation method

作　　者：齐雅楠 康自华 陈婷 杜海军[1] 孙建亮 QI Ya-nan;KANG Zi-hua;CHEN Ting;DU Hai-jun;SUN Jian-liang(School of Chemical Engineering,Guizhou Minzu University,Guiyang 550000,China;School of Electrical and Electronic Engineering,Shandong University of Technology,Zibo 255000,China)

机构地区：[1]贵州民族大学化学工程学院,贵州贵阳550000 [2]山东理工大学电气与电子工程学院,山东淄博255000

出　　处：《现代化工》2023年第5期96-100,105,共6页Modern Chemical Industry

基　　金：贵州省教育厅创新群体重大科研项目(黔教合KY[2018]016);贵州省科技计划项目(黔科合支撑[2020]4Y014,黔科合支撑[2021]一般484,黔科合基础[2020]1Y406);贵州民族大学自然科学类校基金项目(黔科合平台人才[2018]5778-YB20);贵州省高等学校绿色化学与资源环境创新团队(黔教技[2022]13号)。

摘　　要：针对煤化工生产过程中半焦粉煤渣存在多种杂质、阻碍其综合回收和高值化资源利用等问题,利用湿法酸碱调控沉降法工艺制备高纯度氧化铁红,研究了不同固液比、酸浸温度和时间、酸碱度以及煅烧温度和时间对回收率和纯度的影响。结果表明,酸浸过程的最佳制备条件:固液比为1∶6、硫酸浓度为3.68 mol/L、酸浸温度为160℃、酸浸保温时间为4 h;在碱式pH调控沉降体系条件下的最佳制备条件:碱源浓度为2 mol/L、pH为6.8;在煅烧过程中的最佳制备条件:煅烧温度为600℃、煅烧保温时间为2 h。在超声时间为10 min、离心转速为4000 r/min条件下,半焦粉煤渣铁类化合物含铁质量占总质量由24.26%上升为98.12%,氧化铁红产品纯度达98.12%,回收率约为98.69%。In view of the problems such as the existence of various impurities in semi-coke pulverized cinder generated in the coal chemical production process,and difficult comprehensive recovery and utilization of semi-coke pulverized cinder,a wet acid-base regulated sedimentation method is developed to prepare high-purity iron oxide red.The effects of different solid-liquid ratios,acid leaching temperature and time,pH,and calcination temperature and time on iron recovery rate and product purity are studied.The optimum preparation conditions for acid leaching process are determined as follows:the ratio of solid to liquid is 1∶6,the concentration of sulfuric acid is 3.68 mol·L^(-1),the temperature for acid leaching is 160℃,and the holding time for acid leaching is 4 h.The optimum preparation conditions for alkaline pH-regulated sedimentation process are as follows:the concentration of alkali source is 2 mol·L^(-1)and pH is 6.8.The optimum calcination conditions include a calcination temperature of 600℃and a holding time of 2 h.Under 10 min of ultrasonic time and 4000 r·min-1 of centrifugal speed,the iron content of iron compounds in semi-coke pulverized cinder increases from 24.26%to 98.12%,the purity of iron oxide red products reaches 98.12%,and the recovery rate of iron is about 98.69%.

关 键 词：半焦粉煤渣 碱式pH调控沉降体系 氧化铁红 高纯度 铁回收率 

分 类 号：TQ622.15[化学工程—精细化工]