【摘要】 分别以4种离子液体为新型助溶剂,以对甲苯磺酸(Ts OH)和氯磺酸(Cl SO3H)为反应原料,以二氯乙烷为溶剂,制备了对甲苯磺酰氯(Ts Cl)。着重研究了离子液体对Ts OH在二氯乙烷和硫酸中的溶解度比s及Ts Cl产率的影响。研究结果表明,离子液体的加入可显著提高Ts OH的s值,进而提高Ts Cl的产率。在4种离子液体中,[Bu Py]BF4的效果最佳。当[Bu Py]BF4的用量为2(wt)%时,s值和Ts Cl的产率分别达12.5和87.36%。同时,考察了反应物配比、反应温度及反应时间对Ts Cl产率的影响。通过正交实验得到较优的反应条件为:n(Cl SO3H)∶n(Ts OH)为1.5∶1,反应温度为25℃,反应时间为2h。更多还原

【Abstract】 Four kinds of different ionic liquids were investigated as novel co-solvents for synthesis of p-toluene sulfonyl chloride( Ts Cl) with p-toluene sulfonyl acid( Ts OH) and chlorosulfonic acid( Cl SO3H) as feedstocks in ethylidene chloride. The effect of ionic liquids on solubility ratio( s value) of Ts OH in ethylidene chloride and sulphuric acid,as well as the yield of Ts Cl was studied particularly. The results showed that the s value of Ts OH was significantly enhanced with increasing of ionic liquid amount. The yield of Ts Cl thus was also increased,correspondingly. Among four screened ionic liquids,[Bu Py]BF4was proved to be the best co-solvent. The s value of Ts OH and the yield of Ts Cl at optimal [Bu Py]BF4content( 2( wt) %) were 12. 5 and 87. 36%,respectively. The influence of the molar ratio of feedstocks,reaction temperature and reaction time on the yield of Ts Cl were also investigated. The optimum reaction conditions that determined by orthogonal experiment were as follows: n( Cl SO3H)∶ n( Ts OH) = 1. 5∶ 1,reaction temperature is 25℃,reaction time is 2h.更多还原