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针对现行的湿法炼锌渣中提取锗的研究现状,采用新型萃取剂HBL101从锌置换渣的高酸浸出液中直接萃取锗,考察了料液酸度、萃取剂体积分数、萃取温度、萃取时间和相比对萃取的影响以及氢氧化钠质量浓度、反萃温度、反萃时间和反萃相比对反萃的影响,并对萃取剂转型条件进行了研究.实验表明:有机相组成为30%HBL101+70%磺化煤油(体积分数)作为萃取剂,料液酸度为113.2 g·L-1H2SO4,其最佳萃取条件为萃取温度25℃,萃取时间20 min,相比O/A=1∶4.经过五级逆流萃取,锗萃取率达到98.57%.负载有机相用150 g·L-1Na OH溶液可选择性反萃锗得到高纯度锗酸钠溶液,其最佳反萃条件为反萃温度25℃,反萃时间25 min,相比O/A=4∶1.经过五级逆流反萃,反萃率可达到98.1%.反萃锗后负载有机相再用200 g·L-1硫酸溶液反萃共萃的铜并转型,控制反萃温度25℃,反萃时间20 min,O/A=2∶1.经过五级逆流反萃,铜反萃率可达到99.5%并完成转型,萃取剂返回使用.
Aiming at the current research status of extraction of germanium from hydrometallurgical slag, a new extractant HBL101 was used to directly extract germanium from high acid leaching solution of zinc displacement dregs. The effects of acidity, volume fraction of extractant, extraction temperature, extraction time and Compared with the effect of extraction and sodium hydroxide concentration, back-extraction temperature, stripping time and stripping compared to the stripping effect, and the transition conditions were studied.The experimental results show that: the organic phase composition of 30% HBL101 + 70% sulfonated kerosene (volume fraction) as extracting agent, the acidity of feedstock was 113.2 g · L-1H2SO4. The optimum extraction conditions were as follows: extraction temperature 25 ℃, extraction time 20 min, 4. After five-stage countercurrent extraction, the extraction rate of germanium reached 98.57% .When the organic phase was loaded with 150 g · L-1NaOH solution, the stripping of germanium could be selectively stripped to obtain high-purity sodium germanate solution. The optimal stripping conditions were stripping Temperature 25 ℃, stripping time 25 min, compared with O / A = 4:1. After five countercurrent stripping, the stripping efficiency could reach 98.1%. After stripping germanium, the organic phase was loaded with 200 g · L -1 Sulfuric acid solution stripping copper extraction and transformation, the control back-extraction temperature 25 ℃, stripping time 20 min, O / A = 2: 1. After five countercurrent back-extraction, Copper stripping rate of up to 99.5% and complete the transformation, the extractant returned to use.