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4 000 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 4 000 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%.

齐雅楠(1997-),女,硕士研究生,主要从事无机膜分离技术及应用研究,458031702@qq.com。