以对甲基苯硫酚为原料,通过硝化、还原、重氮化等一系列反应合成4-甲基-2-羟基硫酚(A)。考察重氮化过程中NaNO2的用量、硫酸浓度、反应温度以及水解时硫酸浓度对产率的影响。在最佳影响因素下得到最高产率71.2%。通过氯磺化、还原以及最佳反应条件合成含有邻羟基苯硫酚的螯合树脂(B)。使用傅里叶红外光谱表征4-甲基-2-羟基硫酚与螯合树脂。在废旧锂离子电池浸出液中进行分批实验考察4-甲基-2-羟基硫酚与螯合树脂的性能,并且使用HCl溶液提取所螯合的Co2+。研究结果表明:螯合树脂显示良好的可循环性。
4-methyl-2-hydroxythiophenol(A) was synthesized by nitration,reduction and diazotization of p-thiophenol.The influence of dosage of NaNO2,concentration of sulfuric acid,temperature and concentration of H2SO4 in hydrolysis reaction on the yield of 4-methyl-2-hydroxythiophenol was studied.A high yield(71.2%) was achieved under the optimal reaction conditions.And a new chelating resin(B) containing o-hydroxythiophenol was synthesized through chlorosulfonation,reduction and the optimal reactions above.The FT-IR was used to identify the formation of 4-methyl-2-hydroxythiophenol and chelating resin.The adsorption performance of 4-methyl-2-hydroxythiophenol and chelating resin was processed in batch solution which was generated by leaching from LiCoO2,and finally Co2+ was eluted from chelant with HCl solution.Chelating resin displays good recyclability.