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为减少稀土萃取分离废水的处理量,达到节约生产成本的目的,拟寻找出合适的固体皂化剂代替现有的液体皂化技术。对2-乙基己基膦酸单2-乙基己基酯(简称HEH[EHP]或P_(507))为代表的酸性络合萃取剂进行了一系列固体皂化试验,试验结果表明,固体皂化剂MgO与P_(507)完全反应所需的时间最短,为2小时,固体皂化剂NaHCO_3与P_(507)不能完全反应;固体皂化剂MgO、NaHCO_3、Na_2CO_3与P_(507)反应后有机相呈浑浊状态,萃取易发生乳化现象。KOH和K_2CO_3混合固体皂化剂的加入比例和皂化反应温度对皂化性能影响较大,随着KOH百分含量的增加,皂化时间逐渐减少,且在KOH含量为60%时,下降幅度最大;随着反应温度的升高,反应时间逐渐减少;为考察其皂化机理和有机相的萃取性能,对皂化有机相进行了红外光谱分析和饱和萃取容量实验。发现其皂化及萃取机理属于阳离子交换,萃取过程无乳化现象发生,能够达到理论的饱和萃取量。
In order to reduce the amount of wastewater treated by rare earth extraction and separation and achieve the purpose of saving production cost, it is proposed to find a suitable solid saponification agent instead of the existing liquid saponification technology. A series of solid saponification experiments were carried out on the acidic complex extractant represented by 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (abbreviated as HEH [EHP] or P_ (507)). The results showed that the solid saponification agent The time required for the complete reaction of MgO and P_ (507) was the shortest, which was 2 hours. The solid saponifier NaHCO_3 and P_ (507) could not react completely. The organic saponification agent MgO, NaHCO_3, Na_2CO_3 and P_ (507) State, extraction prone to emulsification. The proportion of KOH and K_2CO_3 mixed solid saponifier and the saponification temperature have a great influence on the saponification performance. With the increase of KOH content, the saponification time decreases gradually, and the KOH content is 60% With the increase of reaction temperature and reaction time, the saponification mechanism and the extraction performance of the organic phase were investigated. The infrared spectra and saturation extraction capacity of the saponified organic phase were studied. It was found that the saponification and extraction mechanism belong to the cation exchange, the emulsification phenomenon did not occur during the extraction, and the theoretical saturated extraction capacity could be reached.