漂浮阳极泥富集金银及回收锑铋工艺研究
摘要
漂浮阳极泥是铜电解过程中产生的含砷、锑、铋较高的金银物料,其中含砷13.83%、锑32.67%、铋9.479%、金0.0173%、银0.87%,具有较大的回收价值。
本研究以漂浮阳极泥为原料,采用盐酸浸出富集金银,锑粉还原、两次水解分离锑铋,并用水解分离锑铋产物氯氧锑和氯氧铋分别制备氧化锑和氧化铋。
采用盐酸浸出漂浮阳极泥,当固液比为1：5,反应时间为1h,反应温度为80℃,盐酸浓度为6mol/L时,锑铋浸出率分别可达到99.2%,99.1%。浸出后漂浮阳极泥中金含量为0.26%,银含量为13.12%,与浸出前相比,金银富集15倍以上。
采用过量锑粉还原盐酸浸出液,适宜的锑粉还原条件为：温度60℃,还原时间1～3h。还原液经两次水解分离锑铋,当稀释比为8：1,反应时间为2～3h,反应温度为20℃时,锑水解率可达98.13%。锑水解后液用氢氧化钠调节pH值,进行铋的水解,当温度为20℃,反应时间为1h,终点pH值为3时,铋水解率可达99.5%。
锑水解产物氯氧锑调浆后用碳酸钠溶液转化制备氧化锑,当终点pH值为8.5时,可得到纯度为88.4%,表面形貌为球形的立方晶型的三氧化二锑。
用工业实验所得的铋水解产物粗氯氧铋制备氧化铋,经过盐酸浸出,水解除锑,水解沉铋,氢氧化钠转化,可得到纯度为96.2%的单斜的α—Bi2O3。
漂浮阳极泥富集金银及回收锑铋工艺为漂浮阳极泥的处理开辟了新的思路,可以取得良好的经济效益。
Floating anode slime is Au and Ag samples from copper electrolytic process with high As, Sb, Bi contents, including Asl3.83%, Sb32.67%, Bi9.479%, Au0.0173%, Ag0.87%. So, floating anode slime has a high recovery value.
Hydrochloride acid leaching was utilized to enrich Au and Ag from floating anode slime. Antimony powder reduction, two-step hydrolysises were used to separate Sb and Bi. The hydrolysates SbOC1 and BiOC1 from two-step hydrolysises process were used to prepare Sb2O3 and Bi2O3, respectively.
The leaching rates of Sb and Bi were 99.2% and 99.1% when hydrochloric acid concentration was 6mol/L, reaction temperature was 80℃, ratio of solid to liquid was 1:5, reaction time was 1h. Compared with not-leached floating anode slime, the contents of Au and Ag in leached floating anode slime were enriched more than 15 times.
Antimony powder was used to reduced hydrochloride leaching solution, and the suitable reduction condition was that temperature was 80℃, reaction time was 1～3h. The hydrolysis rate of Sb was 98.13% after the reduction solution was hydrolyzed to separated Sb and Bi, when dilution ratio was 8:1, temperature was 20℃, reaction time was 2～3h. The hydrolysis rate of Bi was 99.5% after the pH of hydrolysis solution of Sb was adjusted to hydrolyze Bi, when temperature was 20℃, reaction time was 1h, final pH was 3.
The Sb2O3 with purity was 88.4%, SEM was spherical and XRD pattern was cubic, was obtained, after the hydrolysate SbOC1 from hydrolysis of Sb was transformed by Na2CO3 to prepare cubic Sb2O3, when the final pH was 8.5.
The Bi2O3 with purity was 96.2%, SEM was fibrous and XRD pattern was monoclinic, was obtained after the crude BiOC1 from industrial experiment was treated by the process of hydrochloride acid leaching, hydrolysis removing Sb, hydrolysis precipitating Bi, NaOH transforming.
The enrichment of Au and Ag and recovery of Sb and Bi from floating anode slime was opened up a new thought for the treatment of floating anode slime, and can acquire good economic benefit.
本研究以漂浮阳极泥为原料,采用盐酸浸出富集金银,锑粉还原、两次水解分离锑铋,并用水解分离锑铋产物氯氧锑和氯氧铋分别制备氧化锑和氧化铋。
采用盐酸浸出漂浮阳极泥,当固液比为1：5,反应时间为1h,反应温度为80℃,盐酸浓度为6mol/L时,锑铋浸出率分别可达到99.2%,99.1%。浸出后漂浮阳极泥中金含量为0.26%,银含量为13.12%,与浸出前相比,金银富集15倍以上。
采用过量锑粉还原盐酸浸出液,适宜的锑粉还原条件为：温度60℃,还原时间1～3h。还原液经两次水解分离锑铋,当稀释比为8：1,反应时间为2～3h,反应温度为20℃时,锑水解率可达98.13%。锑水解后液用氢氧化钠调节pH值,进行铋的水解,当温度为20℃,反应时间为1h,终点pH值为3时,铋水解率可达99.5%。
锑水解产物氯氧锑调浆后用碳酸钠溶液转化制备氧化锑,当终点pH值为8.5时,可得到纯度为88.4%,表面形貌为球形的立方晶型的三氧化二锑。
用工业实验所得的铋水解产物粗氯氧铋制备氧化铋,经过盐酸浸出,水解除锑,水解沉铋,氢氧化钠转化,可得到纯度为96.2%的单斜的α—Bi2O3。
漂浮阳极泥富集金银及回收锑铋工艺为漂浮阳极泥的处理开辟了新的思路,可以取得良好的经济效益。
Floating anode slime is Au and Ag samples from copper electrolytic process with high As, Sb, Bi contents, including Asl3.83%, Sb32.67%, Bi9.479%, Au0.0173%, Ag0.87%. So, floating anode slime has a high recovery value.
Hydrochloride acid leaching was utilized to enrich Au and Ag from floating anode slime. Antimony powder reduction, two-step hydrolysises were used to separate Sb and Bi. The hydrolysates SbOC1 and BiOC1 from two-step hydrolysises process were used to prepare Sb2O3 and Bi2O3, respectively.
The leaching rates of Sb and Bi were 99.2% and 99.1% when hydrochloric acid concentration was 6mol/L, reaction temperature was 80℃, ratio of solid to liquid was 1:5, reaction time was 1h. Compared with not-leached floating anode slime, the contents of Au and Ag in leached floating anode slime were enriched more than 15 times.
Antimony powder was used to reduced hydrochloride leaching solution, and the suitable reduction condition was that temperature was 80℃, reaction time was 1～3h. The hydrolysis rate of Sb was 98.13% after the reduction solution was hydrolyzed to separated Sb and Bi, when dilution ratio was 8:1, temperature was 20℃, reaction time was 2～3h. The hydrolysis rate of Bi was 99.5% after the pH of hydrolysis solution of Sb was adjusted to hydrolyze Bi, when temperature was 20℃, reaction time was 1h, final pH was 3.
The Sb2O3 with purity was 88.4%, SEM was spherical and XRD pattern was cubic, was obtained, after the hydrolysate SbOC1 from hydrolysis of Sb was transformed by Na2CO3 to prepare cubic Sb2O3, when the final pH was 8.5.
The Bi2O3 with purity was 96.2%, SEM was fibrous and XRD pattern was monoclinic, was obtained after the crude BiOC1 from industrial experiment was treated by the process of hydrochloride acid leaching, hydrolysis removing Sb, hydrolysis precipitating Bi, NaOH transforming.
The enrichment of Au and Ag and recovery of Sb and Bi from floating anode slime was opened up a new thought for the treatment of floating anode slime, and can acquire good economic benefit.
引文
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