钛白渣提纯制备电池级硫酸亚铁工艺技术研究
收稿日期: 2019-02-19
网络出版日期: 2020-06-15
基金资助
中低品位磷矿及其共伴生资源高效利用国家重点实验室开放基金课题(WFKF2017-02)
Study on preparation of battery-grade ferrous sulfate by purification of titanium white slag
Received date: 2019-02-19
Online published: 2020-06-15
以某钛白粉生产企业副产钛白渣为原料,选用复合沉淀剂代替传统常用化学沉淀剂,采用一步沉淀法去除杂质,提纯制备电池级高纯硫酸亚铁产品,可作为磷酸铁锂生产原料,为钛白渣的利用提供了新途径。研究结果表明:选用氟化氢铵与还原铁粉按一定质量比配制的复合沉淀剂[m(氟化氢铵):m(还原铁粉)=3.6:1],控制反应条件:反应温度为60 ℃、反应时间为2 h、沉淀剂用量为钛白渣处理量的2.67%(质量分数)、搅拌速度为300 r/min、反应液中Fe2+浓度为1.37 mol/L,最终得到产品纯度为99.98%,镁、钛杂质脱除率均达到99%以上,XRD结果表明产品为七水硫酸亚铁。
郭举 . 钛白渣提纯制备电池级硫酸亚铁工艺技术研究[J]. 无机盐工业, 2019 , 51(8) : 48 -51 . DOI: 10.11962/1006-4990.2018-0675
Battery-grade high-purity ferrous sulphate product was purified and prepared by one-step precipitation method to remove impurities,taking the by-product titanium dioxide slag of a titanium dioxide production enterprise as rawmaterial and using composite precipitator instead of traditional chemical precipitator.It could be used as raw material for lithium iron phosphate production,thus providing a new way for the utilization of titanium white slag.Results showed that the compound precipitator was prepared by mixing ammonium hydrogen fluoride and reduced iron powder in a certain mass ratio of ammonium hydrogen fluoride to reduced iron powder(3.6:1).The reaction conditions were as follows: reaction temperature was 60 ℃, reaction time was 2 h, amount of precipitator was 2.67%(mass fraction) of titanium white slag, stirring speed was 300 r/min and concentration of Fe2+in reaction solution was 1.37 mol/L .The final product purity was 99.98% and the removal rates of Mg and Ti impurities were both over 99%.XRD results showed that the product was ferrous sulfate heptahydrate.
Key words: titanium white slag; ferrous sulfate; purification
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