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鹽酸蒸餾-磷酸三丁酯萃取法從鍺煤煙塵中綜合回收鍺和鎵
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國家自然科學(xué)基金 (U1037603)


Comprehensive Recovery of Germanium and Gallium from Gemanium Coal Dust through Hydrochloric Acid Distillation-Tributyl Phosphate Extraction Process
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    摘要:

    先采用二氧化錳氧化-鹽酸蒸餾提取煤煙塵中的鍺,經(jīng)提純后制備得到高純二氧化鍺,同時煤煙塵中的鎵在蒸餾過程中充分溶解到了鍺蒸餾殘渣液中,過濾后鎵和蒸餾后殘留的鍺進(jìn)入到了蒸餾殘液中,調(diào)節(jié)蒸餾殘液的酸度至5.6 mol/L,采用磷酸三丁酯的260# 溶劑油溶液對鎵進(jìn)行萃取,蒸餾殘液中的少量鍺亦被同時萃取進(jìn)入到有機相中,用氫氧化鈉溶液進(jìn)行反萃取,反萃取完后調(diào)節(jié)pH至6.5~6.7,升溫至85~95 ℃水解,得到氫氧化鎵沉淀和二氧化鍺沉淀,經(jīng)過濾烘干后得到含鍺鎵精礦。鍺的蒸餾回收率可達(dá)到92.37 %以上,殘液中鍺的萃取率可達(dá)到86.18 %以上;鎵的鹽酸浸出率可達(dá)81.23 %以上,鎵的磷酸三丁酯萃取率可達(dá)98.81 %以上,反萃取率可達(dá)99.11 %以上,中和沉淀直收率可達(dá)93.20 %以上;工藝方法具有工藝流程簡短、設(shè)備簡單、過程易于控制,所用生產(chǎn)輔料較少,是一種從煤煙塵中綜合回收鍺和鎵的高效且經(jīng)濟的方法

    Abstract:

    Germanium was extracted from coal dust by manganese dioxide oxidation-hydrochloric acid distillation, and then germanium dioxide with high purity was obtained via purification process. Meanwhile, gallium in the coal dust dissolved fully into germanium distillation residual liquid. After the filtering process, gallium and residual germanium got into the vinasse. The vinasse acidity was adjusted to 5.6 mol/L to extract gallium by 260# solvent oil solution of tributyl phosphate (TBP). A small amount of germanium in the vinasse was extracted as well, and subsequently went into the organic phase. Then sodium hydroxide solution was taken to conduct re-extraction. Afterwards, its pH was adjusted to 6.5~6.7 and it was heated up to 85~95 oC to hydrolyze gallium and germanium. As a result, hydrogen gallium oxide precipitation and germanium dioxide precipitation were produced. Finally germanium and gallium concentrates were obtained via filtering and drying process. By taking the above procedures, the distillation recovery rate of germanium is as high as 92.37%, and the recovery rate of germanium in the vinasse is 86.18%. Hydrochloric acid leaching rate of gallium is above 81.23% and tributyl phosphate recovery rate and re-extraction rate of gallium is 98.81% and 99.11%, respectively. And the neutralized precipitation straight yield rate is 93.20%. Thus, the hydrochloric acid distillation-tributyl phosphate extraction process is a kind of economic and efficient extraction method, enjoying the qualities of short procedures, easier process control, high recovery rate, less time and less assumption of material.

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普世坤,蘭堯中,刀才付.鹽酸蒸餾-磷酸三丁酯萃取法從鍺煤煙塵中綜合回收鍺和鎵[J].稀有金屬材料與工程,2014,43(3):752~756.[Pu Shikun, Lan Yaozhong, Dao Caifu. Comprehensive Recovery of Germanium and Gallium from Gemanium Coal Dust through Hydrochloric Acid Distillation-Tributyl Phosphate Extraction Process[J]. Rare Metal Materials and Engineering,2014,43(3):752~756.]
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  • 收稿日期:2013-03-26
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  • 在線發(fā)布日期: 2014-06-27
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