以高砷精炼铋烟尘为原料制备高纯氯氧化锑

以高砷精炼铋烟尘为原料,采用盐酸浸出、锑粉还原、水解、盐酸溶解、除杂、水解工艺制备高纯氯氧化锑。盐酸浸出高砷精炼铋烟尘,当盐酸溶液与精炼铋烟尘液固比为3：1、反应时间为4 h、反应温度为80℃、盐酸用量为1.2倍理论用量时,Sb,As,Bi和Pb浸出率分别为99.50％,92.79％,95.12％和85.34％;在盐酸浸出液中加入锑粉还原后水解,当水解温度为20℃、水解时间为1 h、稀释比为10：1时,Sb3+水解率达到98.25％;水解产物经盐酸溶解后加入除杂剂,反应1 h后进行二次水解,经过滤、洗涤、烘干所得产品;产品中Sb质量分数达到75.71％,而杂质As,Pb和Bi的质量分数分别为0.081 9％,0.039 2％和0.118 7％。产品为粒度均匀的菱形颗粒,其化学式为SB4O5Cl2。     

采用含砷废水沉淀还原法制备三氧化二砷

介绍以含砷废水为原料采用沉淀还原法制备三氧化二砷.使用氢氧化钠调节含砷废水pH为6,过滤后加入硫酸铜,采用氢氧化钠调节pH为8,经沉淀、过滤、洗涤得到绿色亚砷酸铜粉末.使用水将亚砷酸铜调成浆料,通入SO2还原、过滤、蒸发、冷却结晶得到白色As2O3.实验结果表明:当水与亚砷酸铜液固比(体积与质量比)为4:1 mL/g,还原时间为1 h,还原温度为60℃时,亚砷酸铜中砷浸出率达到89.59%:当还原液pH为0,砷质量浓度为90 g/L,结品温度为28℃时,得到的产物As2O3纯度为95%,As2O3直收率为80.70%,产物质量达到中国有色金属行业标准(YS-T99-1997)中的三级标准.     

漂浮阳极泥中铋的提取与三氧化二铋的制备

漂浮阳极泥经过盐酸浸出、稀释水解、氢氧化钠中和得到氯氧铋,氯氧铋经过氢氧化钠转化制备得到三氧化二铋.当盐酸浓度为6mol/L,固液比为1∶5,反应温度为80℃,反应时间为1h时,漂浮阳极泥中锑和铋浸出率分别达到99.17％和99.08％.当稀释比为8∶1时,盐酸浸出液中锑水解率为98.13％,铋水解率仅为8.8％.稀释后液中加入氢氧化钠溶液,当pH为1.5时,铋水解率达到99.5％,水解产物氯氧铋(BiOCl)中铋、氧、氯的质量分数分别为54.23％,19.30％和14.61％.氯氧铋再次经过盐酸浸出,稀释水解,氢氧化钠沉淀得到氯氧铋.除杂后氯氧铋经过硫酸洗涤、氢氧化钠转化,当氢氧化钠浓度为6mol/L,液固比为3∶1,反应温度为80℃时,反应2h后过滤,用0.5mol/L盐酸洗涤得到形貌为纤维状、晶型为单斜的α-Bi2O3,氧化铋纯度达到99.81％.     

Determination of Dimethylallylamine by Titration in Nonaqueous Solvent

The content of dimethylallylamine was determined using glacial acetic acid as solvent, acetic-formic mixture as an anhydrite, perchloric acid-glacial acetic acid as titrant, and 1% crystal violet in acetic acid as indicator in the presence of methylamine and dimethylamine The influences of inert constituents and water on the titration were investigated, and a complete analytical method was determined. The results showed that the determination error of total amines increased with water increasing, while the effect of water on the determination of dimethylallylamine was little when the amount of water was within 5%, the relative error was generally within 1%, and that the end-point was acutely when about 10% chloroform was added. Compared with gas chromatography, this method is simple, convenient and accurate.     

砷锑价态对铜电解液中砷锑铋脱除率的影响

采用SO2还原,使铜电解液中As(Ⅴ)还原为As(Ⅲ),Sb(Ⅴ)还原为Sb(Ⅲ),并调节电解液中As(Ⅴ)与As(T),Sb(Ⅴ)与Sb(T)的物质的量比,蒸发浓缩电解液,冷却结晶后,能有效脱除铜电解液中As,Sb和Bi等杂质。研究结果表明:当铜电解液体积为3L,Cu的质量浓度为32g/L,As(T)的质量浓度为9.36g/L,Sb(T)的质量浓度为0.65g/L,Bi的质量浓度为0.45g/L,n(As(Ⅴ))/n(As(T))和n(Sb(Ⅴ))/n(Sb(T))分别为0.4时,蒸发浓缩电解液,使浓缩前电解液与浓缩后电解液体积比为2.5,冷却至10℃结晶,过滤,铜电解液中Cu,As,Sb和Bi脱除率分别为82%,62%,55%和85%。蒸发浓缩结晶产物中含CuSO4.5H2O和As2O3。其结晶产物中Cu为29%,As为5%,Sb为0.37%,Bi为0.2%。     

铅锌矿选矿废水的处理及循环利用

采用聚合硫酸铁(PFS)和PFS-FeSO4复合混凝剂处理铅锌矿选矿废水。结果表明:采用PFS处理选矿废水,当剂量(以铁计)为56 mg.L-1时,Cu,Pb和浊度去除率分别可达90.63%,99.97%和100%,但Cr去除率仅为24.98%;采用PFS-FeSO4复合混凝剂处理选矿废水,当剂量(以铁计)分别为42和780 mg.L-1时,Cu和Pb去除率分别为81.25%和99.97%,Cr去除率达到88.74%,但浊度去除率下降至86.06%;当剂量(以铁计)为84 mg.L-1,并在0.5 L废水中加入0.5 g Na2S时,Cu,Pb,Cr和浊度去除率分别为84.69%,99.97%,98.9%和99.14%,去除Cr效果显著增加,处理后选矿废水中的Cu,Pb,Zn和Cr含量低于国家污水综合排放标准(GB8978-1996)。工业放大实验结果表明,处理后废水可循环利用。