富钪锐钛矿浸出液萃取钪钛试验研究

发布时间：2018-11-04 12:07

【摘要】：钪和钛常共同赋存在同一矿物原料、废渣及废液中。所以,在钪的提取过程中进行钛的回收和在钛的提取过程中进行钪的回收都具有重要的现实意义。贵州晴隆富钪锐钛矿原矿含Sc2O3 84.7g/t、Ti02 5.3%,由于锐钛矿嵌布粒度细并组成复杂,钪主要以类质同象型赋存在锐钛矿、褐铁矿、高岭石等矿物中,钪和钛均无法通过常规选矿富集。针对该富钪锐钛矿的开发,拟订了采用“酸浸-萃取”提取钪、钛,并综合回收铁、铝、硅的综合利用方案。论文以硫酸浸出锐钛矿原矿并结晶除铝后的浸出液为研究对象,进行钪和钛的萃取研究,通过单级萃取、反萃,以及三级逆流萃取、反萃的试验研究,确定了“P204优先萃钪-伯胺N1923萃钛”的工艺技术。针对含 H2SO4 360.50g/L,Sc2O313.92mg/L,Ti02 8.29g/L,Fe 25.67g/L 的料液,采用10%P204+5%仲辛醇+260#溶剂油,在O/A=1:6的条件下,经三级逆流萃取,Sc2O3萃取率达98.49%,TiO2萃取率为2.65%,Fe萃取率为0.90%,P204萃钪选择性好;采用3mol/L的NaOH溶液反萃P204负载有机相,在O/A=10:1的条件下,经一级反萃,Sc203反萃率99.94%,得到含Sc2O30.8%的反萃渣,使原矿中的钪富集约95倍,钪的总回收率大于98.43%。P204 萃钪后的料液含 H2SO4315.44g/L,TiO2 7.06g/L,Fe22.26g/L,采用 10%伯胺N1923+5%仲辛醇+260#溶剂油,在O/A=2:1的条件下,经三级逆流萃取,Ti02萃取率达96.18%,Fe萃取率为10.33%,伯胺N1923萃钛效果好;采用3mol/L NH4Cl+1%H2O2反萃伯胺N1923负载有机相,在O/A=2:1的条件下,经三级逆流反萃,Ti02反萃率达99.12%;反萃液经“真空浓缩-冷冻结晶”,NH4Cl结晶循环利用率为60.60%,溶液中Ti02浓度提高到64.06g/L,富集约7倍,钛的总回收率达到91.31%。论文还进行了钪钛共萃取研究,采用10%伯胺N1923+4%P204+5%仲辛醇+260#溶剂油对含 H2SO4360.50g/L,Sc2O313.92mg/L,Ti02 8.29g/L,Fe25.67g/L,的料液三级逆流钪钛共萃,钪萃取率近100%,钛的萃取率为94.93%,共萃效果好,流程短,但反萃困难,有待进一步深入研究。“P204优先萃钪-伯胺N1923萃钛”的工艺技术实现了高酸度硫酸介质中钪、钛的分步提取与富集,工艺流程短,回收率高,富集比大;成功从贵州晴隆富钪锐钛矿中萃取钪、钛,为钪和钛的进一步提取及综合回收铝、铁、硅,实现资源的高效清洁利用奠定基础,并为该类资源的综合利用提供重要参考。论文采用“P204优先萃钪-伯胺N1923萃钛”解决了从高酸度硫酸溶液中依次提取钪钛的技术问题;采用NH4C1+H2O2组合解决了伯胺N1923负载钛有机相反萃困难的技术问题;采用伯胺N1923+P204实现了钪钛共萃;发现了提高硫酸溶液酸度有利于提高P204萃钪选择性的规律。
[Abstract]:Scandium and titanium often occur together in the same mineral raw material, waste residue and waste liquid. Therefore, the recovery of titanium in the extraction process of scandium and the recovery of scandium in the process of extraction of titanium have important practical significance. The anatase ore in Qinglong, Guizhou Province, contains Sc2O3 84.7 g / t Ti02 5.3. Due to the fine granularity and complex composition of anatase, scandium mainly occurs in anatase, limonite, kaolinite and other minerals in the similar synchromatic type, such as anatase, limonite, kaolinite and so on. Both scandium and titanium can not be enriched by conventional dressing. In view of the development of the rich anatase, the comprehensive utilization scheme of extracting scandium and titanium by acid leaching-extraction and comprehensive recovery of iron, aluminum and silicon has been developed. In this paper, the leaching solution of anatase after leaching anatase ore with sulfuric acid as the object of study, the extraction of scandium and titanium was studied, and the experimental study on the extraction of scandium and titanium was carried out by single stage extraction, back extraction, and three stage countercurrent extraction. The technological process of "P 204 preferential extraction of scandium-primary amine N 1923" has been determined. For the feed liquid containing H2SO4 360.50g / L Col _ 2O _ 313.92 mg / L ~ (-1) Ti _ (02) 8.29 g / L ~ (-9) g / L ~ (-1) Fe 25.67g/L, the solvent oil of 10%P204 _ (5%) / octanol 260# was extracted by three-stage countercurrent extraction under the condition of O/A=1:6. The Sc2O3 extraction rate is 98.49% and the extraction rate of TiO2 is 2.65%. The extraction rate of 0.90% is 0.90% and the selectivity of scandium extracted by P204 is good. The organic phase supported on P204 was extracted by NaOH solution of 3mol/L. Under the condition of O/A=10:1, the stripping rate of Sc203 was 99.94%, and the stripping slag containing Sc2O30.8% was obtained, which enriched scandium in raw ore by 95 times. The total recovery rate of scandium was higher than that of 98.43%.P204 extraction solution containing H _ 2SO _ (4315.44) g / L ~ (-1) TIO _ (2) 7.06 g / L Fe _ (22.26) g / L, 10% primary amine N _ (1923)% para-octanol 260# solvent oil was extracted by three-stage countercurrent extraction under the condition of O/A=2:1. The extraction rate of Ti02 is 96.18% and the extraction rate of Fe is 10.33. The primary amine N1923 has good extraction effect. Using 3mol/L NH4Cl 1%H2O2 stripping primary amine N1923 loaded organic phase, under the condition of O/A=2:1, the back extraction rate of Ti02 reached 99.12% after three-stage countercurrent stripping. The recovery rate of NH4Cl was 60.60g / L, the concentration of Ti02 in the solution was increased to 64.06g / L, the concentration of Ti02 was about 7 times, and the total recovery of titanium was 91.31. The co-extraction of scandium and titanium with 10% primary amine N1923 4%P204 5% secondary octanol 260# solvent oil was carried out in this paper. The third stage countercurrent extraction of scandium and titanium containing H _ 2SO _ 4 360.50g / L _ 2C _ 2O _ 3 13.92 mg / L TiTi02 8.29 g / L Fe 25.67 g / L was carried out. The extraction rate of scandium is nearly 100%, the extraction rate of titanium is 94.93%, the extraction effect is good, the process is short, but the back extraction is difficult, so it needs further study. The technology of "P204 preferential extraction of scandium and primary amine N1923 titanium" has realized the Scandium in high acidity sulfuric acid medium. The process of titanium extraction and enrichment is short, the recovery is high and the enrichment ratio is high. The successful extraction of scandium and titanium from Qinglong fulvic anatase in Guizhou laid a foundation for further extraction of scandium and titanium and comprehensive recovery of aluminum, iron and silicon, and provided an important reference for the comprehensive utilization of this kind of resources. In this paper, the technical problem of extracting scandium and titanium sequentially from high acidity sulfuric acid solution was solved by "P204 preferential extraction of scandium and primary amine N1923", and the technical problem of oppositely extracting titanium supported on primary amine N1923 was solved by NH4C1 H2O2 combination. Primary amine N1923 P204 was used to realize the co-extraction of scandium and titanium, and it was found that increasing the acidity of sulfuric acid solution was beneficial to the improvement of selectivity of scandium.
【学位授予单位】：昆明理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TD95

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