提高钼冶炼废酸中钼离子交换吸附性能的研究
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摘要
开展了采用石灰适度中和的方法,改善钼冶炼废酸中钼吸附性能的研究。主要进行了石灰加入量、反应温度、反应时间等预处理条件试验,对滤渣的组成进行了X射线衍射仪(XRD)表征,并对预处理前后的钼冶炼废酸进行了静态、动态吸附试验。试验结果表明:石灰加入量小于75 g·L~(-1)条件下,预处理过程钼铼损失率较低; CaO加入量为50 g·L~(-1),反应温度25℃,反应时间100 min条件下,废酸中硫、氟和硅的脱除率分别为66.16%, 0.21%和9.65%,相比于未处理废酸,上述条件下预处理后废酸进行离子交换吸附时,铼的静态平衡吸附容量从11.36 mg·ml~(-1)提高到13.53 mg·ml~(-1),钼的静态平衡吸附容量由20.25 mg·ml~(-1)提高到147.63 mg·ml~(-1);采用D314树脂在1 BVs流速下对钼进行动态吸附,处理液量在120 BV时,C/C_0=0.3,吸附效果较好;采用10%的氨水溶液在0.5 BVs流速下解吸附,解吸液含钼39.25 g·L~(-1),钼得到有效富集。
Research on improving the ion-exchange adsorption performance of Mo in spraying water by moderate neutralization method was discussed, additionally lime was used as neutralizing agent. A series of experiments were done at different condition of lime amount, reaction temperature and reaction time etc. The residues were characterized by X-ray diffraction(XRD). The spraying water before and after pretreatment by lime was used for adsorption experiments respectively and the differences of ion-exchange performance of Mo was compared. Results showed loss ratio of Re and Mo in pretreatment process was very low when the lime amount added in the spraying water was less than 75 g·L~(-1). In the pretreatment process the removal rate of S, F and Si was 66.16%, 0.21% and 9.65% respectively under the optimum conditions including lime amount of 50 g·L~(-1), reaction temperature of 25 ℃, reaction time of 100 min. At the same experimental conditions, the static equilibrium adsorption capacity of Re was increased from 11.36 to 13.53 mg·ml~(-1) and the static equilibrium adsorption capacity of Mo was increased from 20.25 to 147.63 mg·ml~(-1), when the resin was put in the spraying water after pretreatment. The dynamic adsorption experiments, D314 resin was used as adsorbent and the flow rate was 1 BV·h~(-1), showed that C/C_0=0.3 when the volume of effluent was 120 BV, which meant that the absorbing effect of Mo was satisfied. Desorption solution, in which the content of Mo was 39.25 g·L~(-1), was gained by the condition that the eluting agent of 10% ammonia, flow rate of 0.5 BV·h~(-1). Mo in the spraying water was enriched effectively.
Research on improving the ion-exchange adsorption performance of Mo in spraying water by moderate neutralization method was discussed, additionally lime was used as neutralizing agent. A series of experiments were done at different condition of lime amount, reaction temperature and reaction time etc. The residues were characterized by X-ray diffraction(XRD). The spraying water before and after pretreatment by lime was used for adsorption experiments respectively and the differences of ion-exchange performance of Mo was compared. Results showed loss ratio of Re and Mo in pretreatment process was very low when the lime amount added in the spraying water was less than 75 g·L~(-1). In the pretreatment process the removal rate of S, F and Si was 66.16%, 0.21% and 9.65% respectively under the optimum conditions including lime amount of 50 g·L~(-1), reaction temperature of 25 ℃, reaction time of 100 min. At the same experimental conditions, the static equilibrium adsorption capacity of Re was increased from 11.36 to 13.53 mg·ml~(-1) and the static equilibrium adsorption capacity of Mo was increased from 20.25 to 147.63 mg·ml~(-1), when the resin was put in the spraying water after pretreatment. The dynamic adsorption experiments, D314 resin was used as adsorbent and the flow rate was 1 BV·h~(-1), showed that C/C_0=0.3 when the volume of effluent was 120 BV, which meant that the absorbing effect of Mo was satisfied. Desorption solution, in which the content of Mo was 39.25 g·L~(-1), was gained by the condition that the eluting agent of 10% ammonia, flow rate of 0.5 BV·h~(-1). Mo in the spraying water was enriched effectively.
引文
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[12] Jiang C J.Existing Forms and Adsorption Behavior on Ion Exchange Resin of Mo(VI) in Acidic Sulfate Solution [D].Changsha:Central South University,2014.16.(蒋长俊.酸性硫酸盐溶液体系中Mo(VI)的存在形态与其离子交换树脂吸附行为 [D].长沙:中南大学,2014.16.)
[13] Dean J A.Langes Chemistry Handbook [M].Beijing.Science Press,1991.5.(迪安 J A主编.兰氏化学手册 [M].北京:科学出版社,1991.5.)
[14] Song Y L,Dong Z J.Rare Metal Chemistry [M].Shenyang:Liaoning University Press,1994.239.(宋玉林,董贞俭.稀有金属化学 [M].沈阳:辽宁大学出版社,1994.239.)
[15] Peng C H,Tong Z Q.Study on the oxidation of calcium sulfite to gypsum [J].Journal of China Institute of Metrology,2002,13(2):139.(彭朝辉,童志权.亚硫酸钙氧化为石膏的研究 [J].中国计量学院学报,2002,13(2):139.)
[2] Zou Z Q,Zhou Q J.Recovery of molybdenum and rhenium from molybdenite concentrate in dexing copper ore by lime roasting-N235 extraction method [J].Mining and Metallurgical Engineering,2002,22(2):79.(邹振球,周勤俭.钼精矿石灰焙烧-N235萃取工艺提取钼铼 [J].矿冶工程,2002,22(2):79.)
[3] Vartak S V,Shinde V M.Separation studies of molybdenum(VI) and rhenium(VII) using TPPO as an extractant [J].Talanta,1996,43(9):1465.
[4] Zhang Y Z.Extraction and Analysis of Rhenium from Copper Smelting Waste Acid [D].Hefei:Hefei University of Technology,2011.15.(张永中.铜冶炼废酸提取铼及分析方法的研究 [D].合肥:合肥工业大学,2011.15.)
[5] Li Y P,Li L F,Wang X K.Extraction of high purity rhenium using liquid membrane method [J].China Molybdenum Industry,2001,25(6):23.(李玉萍,李莉芬,王献科.液膜法提取高纯铼 [J].中国钼业,2001,25(6):23.)
[6] Seo S Y,Choi W S,Yang T J,Kim M J,Tran T.Recovery of rhenium and molybdenum from a roaster fume scrubbing liquor by adsorption using activated carbon [J].Hydrometallurgy,2012,129-130(3):145.
[7] Mozammel M,Sadrnezhaad S K,Badami E,Ahmadi E.Breakthrough curves for adsorption and elution of rhenium in a column ion exchange system [J].Hydrometallurgy,2007,85(1):17.
[8] Liu Y,Deng L,Liu L,Zhou Y Z,Chang Y L.Adsorption of Re from electrolyte of superalloy by using D296 resin [J].Chinese Journal of Rare Metals,2017,41(6):678.(刘洋,邓丽,刘莉,周亦胄,常云龙.D296树脂对高温合金电解液中Re的吸附研究 [J].稀有金属,2017,41(6):678.)
[9] Li H G.Application of ion-exchange process in rhenium recovery [J].China Molybdenum Industry,1995,19(1):18.(李洪桂.离子交换技术在铼回收过程中的应用 [J].中国钼业,1995,19(1):18.)
[10] Liu H Z,Wang L J,Zhang B,Wang W.Static adsorption properties of a kind of weak anion ion resin for rhenium in spraying water [J].Chinese Journal of Rare Metals,2017,41(9):1028.(刘红召,王力军,张博,王威.一种弱碱性树脂对淋洗液中铼的静态吸附性能 [J].稀有金属,2017,41(9):1028.)
[11] Jiang K X,Deng G C,Zhang Q,Zhang J,Zhai Y C.Experimental research on the static separation of rhenium from molybdenum with D314 resin [J].Rare Metals and Cemented Carbides,2011,39(1):8.(蒋克旭,邓桂春,张倩,张俊,翟玉春.D314树脂静态分离铼与钼的实验研究 [J].稀有金属与硬质合金,2011,39(1):8.)
[12] Jiang C J.Existing Forms and Adsorption Behavior on Ion Exchange Resin of Mo(VI) in Acidic Sulfate Solution [D].Changsha:Central South University,2014.16.(蒋长俊.酸性硫酸盐溶液体系中Mo(VI)的存在形态与其离子交换树脂吸附行为 [D].长沙:中南大学,2014.16.)
[13] Dean J A.Langes Chemistry Handbook [M].Beijing.Science Press,1991.5.(迪安 J A主编.兰氏化学手册 [M].北京:科学出版社,1991.5.)
[14] Song Y L,Dong Z J.Rare Metal Chemistry [M].Shenyang:Liaoning University Press,1994.239.(宋玉林,董贞俭.稀有金属化学 [M].沈阳:辽宁大学出版社,1994.239.)
[15] Peng C H,Tong Z Q.Study on the oxidation of calcium sulfite to gypsum [J].Journal of China Institute of Metrology,2002,13(2):139.(彭朝辉,童志权.亚硫酸钙氧化为石膏的研究 [J].中国计量学院学报,2002,13(2):139.)
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