氯铝酸离子液体催化合成t-BAMBP

Synthesis of t-BAMBP in Chloride-Aluminium(Ⅲ) Chloride Ionic Liquids

4-叔丁基-2-(α-甲基苄基)苯酚(t-BAMBP)是分离纯化Rb和Cs的萃取剂,应用t-BAMBP的萃取色谱法分离流程简便、高效,对Cs的去污系数大于106,Rb的化学回收率大于80%。以前t-BAMBP的合成方法是以对叔丁基苯酚和苯乙烯为起始原料,Lewis酸催化。为了改进反应条件,提高产率,以对叔丁基苯酚和苯乙烯为起始原料,以氯铝酸离子液体作催化剂,合成了t-BAMBP。通过对此烷基化反应的研究,考察了离子液体的组成和用量、反应时间、反应温度以及反应物配比等主要参数对t-BAMBP生成的影响,结果表明,氯铝酸离子液体([BuMeI m]Br-AlCl3)对合成t-BAMBP的烷基化反应具有良好的催化作用;最佳反应条件为:反应物4-特丁基苯酚和苯乙烯摩尔比为1∶1.2,离子液体催化剂的组成x(AlCl3)=0.67,离子液体用量为1∶0.10(4-特丁基苯酚/离子液体摩尔比),加热60℃以上反应5 min;在最佳反应条件下,t-BAMBP的产率可达40.6%。

The 4-tert-butyl-2-（α-methylbenzyl ） phenol （t-BAMBP） is used for the separa- tion of Rb and Cs by means of extraction-chromatography. The radiochemical separation proeedure of Rb is simple and efficient. Decontamination factor for Cs is more than 106, and recovery ratio for Rb is more than 80 %. Traditionally, the t-BAMBP was synthesized based on p-tert-butylphenol and styrene as raw material, Lewis acid as catalyst. In order to improve the reactive condition and increase the yield of t-BAMBP, the ionic liquid, chloridealuminium （Ⅲ） chloride, was used as catalyst. The alkylation had been investigated, and higher conversion was obtained. The effects of catalyst composition and quantity, reaction temperature and time, ration of reactant were studied. The results show that the ionic liquids have better catalytic performance for the title reaction. The optimal synthetical conditions are as follows： in the reaction, the mole fraction of x（AlCl3 ） in ionic liquid is 0.67, the mole ratio of ionic liquid is 1 ＂ 0. 10 （4-tert-butylphenol/eatalyzer）, the reaction time is 5 rain, the reaction tempera- ture is above 60 ℃ and the mole ratio of reactants is 1 ： 1.2（4-tert-butylphenol/styrene）. At the optimum conditions, yield of t-BAMBP is 40. 6 %.