【作者】 苏文征；

【导师】 周志明；

【作者基本信息】 重庆大学 ， 化学工程， 2006， 硕士

【摘要】 富锰渣是由贫锰矿富集得到的,其锰含量约为35%～45%,我国富锰渣年产量在20～25万吨,目前主要是作为冶炼锰铁合金的原料。由于其用途单一,易受到铁合金行业市场波动的影响。为拓展富锰渣的利用途径,本文对以富锰渣为原料、盐酸作浸出剂,经酸浸、除杂、结晶、干燥制备无水氯化锰的工艺进行了探索。对酸浸过程,主要研究了浸出时间、浸出温度、盐酸浓度和用量对浸出的影响。研究表明:①在正交试验设计水平条件下,上述因素对锰的浸出率产生影响的大小顺序为:浸出温度>盐酸浓度>盐酸用量>浸出时间;②当控制浸出条件为:盐酸浓度2mol/L、浸取时间1h、反应温度25℃、盐酸用量为理论用量的180%时,锰的最佳浸出率为87.74%。除杂操作中,对铁的分离、中和剂的选择、锰、镁的溶剂萃取分离工艺进行了探索。结果表明:①酸浸液中Fe²⁺经MnO₂于80℃氧化成Fe³⁺,Fe³⁺可用0.9mol/L的P204煤油溶液于常温、O/A=10:1、萃取时间=20min条件下经单级萃取Fe³⁺的萃取率为99.4%,萃余相中[Fe³⁺]<1.0×10-5mol/L。负载有机相经浓盐酸反萃后可再生回用。②选择碳酸锰作中和剂;③Ca²⁺用硫酸锰进行沉淀分离;④在酸浸液PH≈1.8,温度为50～60℃,以硫化钠沉淀重金属;⑤选用0.9mol/L的P204煤油溶液,控制萃取温度为25℃、萃取时间为20min,采用三级逆流萃取可实现锰、镁的分离,平均分离系数约为47.23。负载有机相可用2mol/L盐酸反萃再生。净化液经浓缩结晶干燥可制得无水氯化锰产品,其中氯化锰含量为95.10%,产品符合工业氯化锰要求,锰的总收率达到79.3%。更多还原

【Abstract】 Rich-manganous slags are enriched from poor-manganous mineral, and the content of manganese is about 35%⁴5%. The output of rich-manganous slags, the main material of smelting manganese-iron alloy these years, is 200²50 kt in our country. For its single use, rich-manganous slags are liable to the fluctuant market of iron alloy industry. To developing the use of rich-manganous slags, this article discussed the technology of preparing manganese chloride by using rich-manganous slags as feed stock, hydrochloric acid as leaching solvent, and through pickling, impurity removing, crystallization and drying.In the process of pickling, it was studied the effect of leaching time and temperature, concentration and dosage of hydrochloric acid on leaching rate. The result shows:①Based on the orthogonality experiments, the sequence of all factors that affect the leaching rate is: temperature> HCl concentration> HCl dosage> leaching time;②The highest leaching rate of manganese is 87.74%, when HCl concentration is 2mol/L, leaching time 1h, temperature 25℃and HCl dosage 1.8 times as much as theory.In the operation of impurity removing, feasibility of iron separation was studied, so as selecting of neutralizer and precipitant, the method of manganese or magnesium separation by solvent extraction. It concluded:①Pickling solution was oxidated enough by MnO2 at 80℃, Fe³⁺ could be completely extracted for 20 minutes at room temperature by 0.9mol/L P204 dissolved in kerosene. It also could be hydrolyzed and then precipitated with aluminum（pH=5⁶）;②Manganese carbonate was selected as neutralizer;③Ca²⁺ could be precipitated by manganese sulfate;④heavy metal could be precipitated at pickling solution pH≈1.8, temperature 50～60℃and sodium sulfide as vulcanization precipitant;⑤Acidic extractant P204 is suitable for extracting manganese and magnesium. Separating Mn and Mg could be operated for 20 minutes at 25℃with 0.9mol/L P204 dissolved in kerosene by multistage counter-current extraction method. The average separation coefficient was 47.23, and the loading organic phase could be reconstituted by stripping with 2mol/L HCl.The manganese chloride could be obtained by concentrating, crysaling and drying decontaminated solution, in which the content of manganese chloride is 95.10%. The product could achieve industrial level.更多还原