氟硅酸处理含钾页岩中硅铝铁的高效分离技术研究

发布时间：2018-05-03 07:49

  本文选题：含钾页岩 + 铁铝分离　； 参考：《贵州大学》2015年硕士论文

【摘要】：含钾页岩是一种难溶性的含钾矿物,富含K2O在9%左右,储量丰富,品质优良,且分布广泛,我国从20世纪50年代,就开始研究和开发利用不溶性钾矿制备钾肥。贵州省就有近百个含钾岩石的矿点,矿产储存量很大,仅铜仁矿带的储量就超过50亿吨。本文所述含钾页岩是以贵州铜仁市万山特区的钾页岩为研究对象,采用化学分析和XRD分析,得到其主要化学成分为K2O、SiO2、Al2O3,三者含量之和大于85%。本文主要研究的是氟硅酸分解含钾页岩后的固体(以下称为固体溶样),探讨了其中硅铝铁的提取和分离方法。本实验选用浓硫酸将固体溶样中的氟和硅挥发掉,将铁铝转变为可溶性的盐。原矿粉质量(g):硫酸用量(ml)为1:0.6时,中间体铝的提取率可达95.3%,铁的提取率可达到86.8%。当溶解用水的体积(ml)和洗水的体积(ml)分别为矿粉质量(g)的4倍和1倍时,能够将可溶性的硫酸铁和硫酸铝完全溶解。本实验采用三级有机络合沉淀分离铁铝,单因素实验确定最佳工艺条件为:一级分离过程:铁与DDTC的质量比为1:8,溶液pH为1.8,反应温度35℃,反应时间为10min,溶液中铁的分离率为74.6%。二、三级分离过程:铁与DDTC的质量比为1:10,溶液pH为1.8,反应温度25℃,反应时间为5min,溶液中铁的分离率为99%。经过三级分离溶液中铁的分离率可以达到99%。铁的络合物可以与碱反应制备氢氧化铁,经过煅烧后得到氧化铁。通过单因素实验确定最佳工艺条件为:Fe-DDTC与KOH的固液比为1:50,反应温度60℃,反应时间2h,聚乙二醇加入量为3ml时,制备的氧化铁的纯度为91.2%。氧化铝制备过程,通过单因素实验确定的最佳反应工艺条件是,反应温度60℃,反应时间0.5h,反应体系的pH为8,氨水的质量分数为15%时,制备的氧化铝的纯度为92.3%。
[Abstract]:Potash shale is an insoluble mineral containing potassium, rich in about 9% of K 2O, rich in reserves, excellent quality and widely distributed. In China, insoluble potassium ore has been studied and utilized to produce potassium fertilizer since 1950s. Guizhou province has nearly 100 K-bearing rock ore sites, the mineral reserves are very large, Tongren ore belt alone reserves more than 5 billion tons. In this paper, the potassium shale in Wanshan Special Zone of Tongren City, Guizhou Province is taken as the research object. By chemical analysis and XRD analysis, the main chemical composition of the shale is K _ 2O _ 2O _ 2 Sio _ 2 and Al _ 2O _ 3, and the sum of the three contents is more than 85%. In this paper, the method of extraction and separation of silicon-aluminum-ferric acid from the solid after the decomposition of potassium shale by fluorosilicic acid (hereinafter referred to as solid dissolved sample) is studied. In this experiment, concentrated sulfuric acid was used to volatilize the fluorine and silicon in the solid sample, and to transform iron and aluminum into soluble salt. When the mass of raw ore powder is 1: 0.6, the extraction rate of aluminum and iron can reach 95.3and 86.8 respectively. When the volume of dissolved water (ml) and the volume of washing water (ml) are 4 times and 1 times of the mass of mineral powder, the soluble ferric sulfate and aluminum sulfate can be dissolved completely. In this experiment, the three-stage organic complexation precipitation was used to separate iron and aluminum. The optimum technological conditions were determined as follows: the mass ratio of iron to DDTC was 1: 8, the pH of solution was 1.8, the reaction temperature was 35 鈩，

本文编号：1837637