【摘要】：鈧和鈦常共同賦存在同一礦物原料、廢渣及廢液中。所以,在鈧的提取過(guò)程中進(jìn)行鈦的回收和在鈦的提取過(guò)程中進(jìn)行鈧的回收都具有重要的現(xiàn)實(shí)意義。貴州晴隆富鈧銳鈦礦原礦含Sc2O3 84.7g/t、Ti02 5.3%,由于銳鈦礦嵌布粒度細(xì)并組成復(fù)雜,鈧主要以類質(zhì)同象型賦存在銳鈦礦、褐鐵礦、高嶺石等礦物中,鈧和鈦均無(wú)法通過(guò)常規(guī)選礦富集。針對(duì)該富鈧銳鈦礦的開(kāi)發(fā),擬訂了采用“酸浸-萃取”提取鈧、鈦,并綜合回收鐵、鋁、硅的綜合利用方案。論文以硫酸浸出銳鈦礦原礦并結(jié)晶除鋁后的浸出液為研究對(duì)象,進(jìn)行鈧和鈦的萃取研究,通過(guò)單級(jí)萃取、反萃,以及三級(jí)逆流萃取、反萃的試驗(yàn)研究,確定了“P204優(yōu)先萃鈧-伯胺N1923萃鈦”的工藝技術(shù)。針對(duì)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#溶劑油,在O/A=1:6的條件下,經(jīng)三級(jí)逆流萃取,Sc2O3萃取率達(dá)98.49%,TiO2萃取率為2.65%,Fe萃取率為0.90%,P204萃鈧選擇性好;采用3mol/L的NaOH溶液反萃P204負(fù)載有機(jī)相,在O/A=10:1的條件下,經(jīng)一級(jí)反萃,Sc203反萃率99.94%,得到含Sc2O30.8%的反萃渣,使原礦中的鈧富集約95倍,鈧的總回收率大于98.43%。P204 萃鈧后的料液含 H2SO4315.44g/L,TiO2 7.06g/L,Fe22.26g/L,采用 10%伯胺N1923+5%仲辛醇+260#溶劑油,在O/A=2:1的條件下,經(jīng)三級(jí)逆流萃取,Ti02萃取率達(dá)96.18%,Fe萃取率為10.33%,伯胺N1923萃鈦效果好;采用3mol/L NH4Cl+1%H2O2反萃伯胺N1923負(fù)載有機(jī)相,在O/A=2:1的條件下,經(jīng)三級(jí)逆流反萃,Ti02反萃率達(dá)99.12%;反萃液經(jīng)“真空濃縮-冷凍結(jié)晶”,NH4Cl結(jié)晶循環(huán)利用率為60.60%,溶液中Ti02濃度提高到64.06g/L,富集約7倍,鈦的總回收率達(dá)到91.31%。論文還進(jìn)行了鈧鈦共萃取研究,采用10%伯胺N1923+4%P204+5%仲辛醇+260#溶劑油對(duì)含 H2SO4360.50g/L,Sc2O313.92mg/L,Ti02 8.29g/L,Fe25.67g/L,的料液三級(jí)逆流鈧鈦共萃,鈧萃取率近100%,鈦的萃取率為94.93%,共萃效果好,流程短,但反萃困難,有待進(jìn)一步深入研究�！癙204優(yōu)先萃鈧-伯胺N1923萃鈦”的工藝技術(shù)實(shí)現(xiàn)了高酸度硫酸介質(zhì)中鈧、鈦的分步提取與富集,工藝流程短,回收率高,富集比大;成功從貴州晴隆富鈧銳鈦礦中萃取鈧、鈦,為鈧和鈦的進(jìn)一步提取及綜合回收鋁、鐵、硅,實(shí)現(xiàn)資源的高效清潔利用奠定基礎(chǔ),并為該類資源的綜合利用提供重要參考。論文采用“P204優(yōu)先萃鈧-伯胺N1923萃鈦”解決了從高酸度硫酸溶液中依次提取鈧鈦的技術(shù)問(wèn)題;采用NH4C1+H2O2組合解決了伯胺N1923負(fù)載鈦有機(jī)相反萃困難的技術(shù)問(wèn)題;采用伯胺N1923+P204實(shí)現(xiàn)了鈧鈦共萃;發(fā)現(xiàn)了提高硫酸溶液酸度有利于提高P204萃鈧選擇性的規(guī)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.
【學(xué)位授予單位】：昆明理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TD95

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本文編號(hào)：2309771