湿法冶炼冶金用硅

N. Nemchinova, A. Tyutrin, A. Zaitseva
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摘要

本文介绍了用无机酸浸出杂质精制冶金级硅的结果。采用金相分析、x射线荧光分析和x射线光谱显微分析方法对硅样品进行了研究。为提高该合金元素的质量,采用不同酸(10 % H2SO4、HCl、HNO3、4 % HF)及其混合物对其进行了湿法冶金净化实验。计算了所研究的硅样品(FeSi2、Fe2Si、FeSi、AlFeSi、AlFeSi2、Al3FeSi2、FeSi2Ti、FeAlTiSi、TiSi2、Ca2Si)中主要杂质夹杂物与试剂相互作用反应的吉布斯能变化值。实验以粒径为-200 μm的硅样品为对象,在温度为60 °С,持续时间为1 h, L:S = 5:1的条件下,用磁力搅拌器不断搅拌。采用原子发射法测定浸出后溶液中杂质元素的浓度。以氢氟酸为溶剂提纯铁、铝和钛的效果最好(溶液浓度,分别为:2380、831、145 mg/dm3)。细硅经盐酸处理后,溶液中钙的最大浓度为147 mg/dm3。将杂质转移到溶液中最有效的方法是将硫酸和氢氟酸按1:1的比例混合。使用H2SO4和HCl的混合物作为溶剂(比例为1:3)可以在浸出液中获得足够高的杂质元素质量浓度。从铁、铝、钙、钛中提纯硅的比例分别为33.32%、54.64%、65.77%和15.64%。
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Hydrometallurgical refining of metallurgical silicon
The paper presents the results of refining silicon of metallurgical grades based on leaching of impurities with inorganic acids. Silicon samples were studied by metallographic and X-ray fluorescent methods of analysis, as well as X-ray spectral microanalysis. To improve the quality of this alloying element, we carried out experimental work on its hydrometallurgical purification with solutions of various acids (10 % H2SO4 , HCl, HNO3 , 4 % HF) and their mixtures. Values of changes in the Gibbs energy were calculated for reactions of interaction with reagents of the main impurity inclusions recorded in the studied silicon samples (FeSi2 , Fe2Si, FeSi, AlFeSi, AlFeSi2 , Al3FeSi2 , FeSi2Ti, FeAlTiSi, TiSi2 , Ca2Si). The experiments were carried out on silicon samples with a particle size of –200 μm with constant stirring by a magnetic stirrer at a temperature of 60 °С, duration 1 h and L:S = 5:1. Determination of concentration of the impurity elements in the solution after leaching was made by the atomic emission method of analysis. When hydrofluoric acid is used as a solvent, the best results are obtained for purification of iron, aluminum, and titanium (concentration in solution, mg/dm3, respectively: 2380, 831, 145). The maximum concentration of calcium in the solution (147 mg/dm3 ) was achieved by hydrochloric acid treatment of fine silicon. The most effective for transferring impurities into solution is a mixture of sulfuric and hydrofluoric acids at a ratio of 1:1. Using a mixture of H2SO4 and HCl as a solvent (at a ratio of 1:3) made it possible to achieve sufficiently high mass concentrations of impurity elements in the leaching solution. The degree of silicon purification from iron was 33.32 %, aluminum – 54.64 %, calcium – 65.77 %, titanium – 15.64 %.
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