居中军，王成彦，尹 飞，杨永强，李敦钫

(北京矿冶研究总院 冶金研究设计所，北京 100070)

石煤钒矿硫酸活化常压浸出提钒工艺

居中军，王成彦，尹 飞，杨永强，李敦钫

(北京矿冶研究总院 冶金研究设计所，北京 100070)

研究石煤钒矿的硫酸活化提钒方法。分别考察矿石粒度、硫酸浓度、活化剂用量、催化剂用量、反应温度、反应时间和浸出液固比等因素对钒浸出率的影响。结果表明：石煤提钒的优化条件为矿石粒度小于74 μm的占80%、硫酸浓度150 g/L、活化剂CaF2用量(相对于矿石)60 kg/t、催化剂R用量20 g/L、反应温度90 ℃、反应时间6 h、液固比(体积/质量，mL/g)2:1，在此优化条件下，钒浸出率可达94%以上；在优化条件下，采用两段逆流浸出，可有效减少活化剂CaF2以及浸出剂硫酸的消耗量；经过两段逆流浸出−萃取−反萃−氧化水解工艺，全流程钒资源总回收率可达86.9%；V2O5产品纯度高于99.5%。

石煤；钒；活化酸浸；活化剂；浸出率

Abstract:The method of activated sulfuric acid leaching of stone coal vanadium ore was studied. The effects of the ore particle sizes, sulfuric acid concentration, amount of active agent and catalyst agent, reaction temperature, reaction time and liquid to solid ratio on the leaching rate of vanadium were investigated, respectively. The results show that the optimal conditions of leaching vanadium from stone coal are as follows: stone coal with size less than 74 μm accounting for 80%, sulfuric acid concentration 150 g/L, dosage of active agent (relative to ore) CaF260 kg/t, dosage of catalyst R 20 g/L, reaction temperature 90 ℃, reaction time 6 h and liquid to solid ratio (volume/mass, mL/g) 2:1. Under the best condition, the leaching rate of vanadium can be higher than 94%. Under the optimum condition, the two-stage counter-current leaching process was employed, and the dosages of sulfuric acid and active agent CaF2can be saved. The total recovery rate of vanadium is 86.9% throughout the whole process of two-stage counter-current leaching−solvent extraction−stripping−oxydrolysis. The purity of product V2O5is higher than 99.5%.

Key words:stone coal; vanadium; activated acid leaching; active agent; leaching rate

自然界中钒矿主要有钒钛磁铁矿和石煤钒矿，我国拥有丰富的石煤钒矿资源，主要集中在四川、湖南、湖边、甘肃和贵州等地，全国石煤储量为618.8亿t，蕴藏于石煤中的V2O5储量为11 797万t，其中V2O5品位≥0.5%的资源储量为7 707.5万t，是我国钒钛磁铁矿中V2O5储量的2.7倍[1]。以上数据显示，我国的石煤钒矿具有很高的工业价值。

目前，应用较广的石煤钒矿提钒工艺主要是采用钠化焙烧−水浸−铵盐沉钒工艺流程[2−4]，该工艺首先在氯化钠存在的条件下于800～850 ℃焙烧2～2.5 h，使使石煤钒矿中的 V(Ⅲ)及 V(Ⅵ)转化为可溶性的钒酸钠，焙砂经过水浸得到钒酸钠溶液，然后采用铵盐沉钒的方式得到钒酸氨渣，煅烧钒酸铵渣可得到粗V2O5产品。……