从废旧高温合金中提取Re的试验研究

Experimental Study on Rhenium Extraction from Waste Superalloy

针对高温合金高致密性、难溶解的特点,采用真空气雾化法将废旧高温合金制成活性很高的细微颗粒,再经氧化酸浸后,废旧高温合金粉中的Re以ReO-4形态进入溶液,Re浸出率达99.02%;酸浸液用NaOH饱和溶液调pH值至1.5后,用D296型阴离子交换树脂吸附Re,Re吸附率达98.76%;解吸过程中先用NH3·H2O+NH4Cl混合溶液解吸D296负载树脂上的Mo,Re损失率为4.97%,再用NH4SCN溶液解吸Re,Re解吸率达94.98%;含Re解吸后液可通过添加KCl或NH4Cl蒸发浓缩冷却结晶工序制备含Re产品,控制浓缩液中Re浓度大于22.38g/L,Re结晶率可达90%以上。X射线荧光光谱分析结果表明,所获得的KReO4和NH4ReO4产品纯度分别达到了99.21%和99.58%。

According to the characteristics of high density and insolubility of superalloy,fine particles with high activity were prepared from waste superalloy by vacuum atomization.Rhenium in waste superalloy powder was dissolved into solution in the form of ReO4^- after oxidation acid leaching.And Re leaching rate reaches 99.02%.Subsequently,the pH value of the acid leaching solution was adjusted to 1.5with saturated NaOH solution,and then rhenium was adsorbed onto D296 anion exchange resin.And Re adsorption rate reaches 98.76%.During the process of desorption,Mo loaded in the D296 resin was preferentially desorbed with the mixed solution of ammonia and ammonium chloride,with Re loss rate of 4.97%.Rheniumwas desorbed with ammonium thiocyanate solution,with Re desorption rate of 94.98%.The Re-containing products were prepared from the desorbed solution containing rhenium by adding KCl or NH4Cl and evaporation cooling crystallization.Re crystallization rate is higher than 90% by controlling the rhenium concentration over 22.38g/L in concentrated solution.The results of X-ray fluorescence analysis show that the purity of potassium rhenate and ammonium rhenate reaches 99.21% and 99.58%,respectively.