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采用DMF钝化氯磺酸活性的方法开发了一种对同时含有醇羟基和芳香环的有机原料实现高选择性硫酸酯化的方法。运用该技术以壬基酚聚氧丙烯醚(NPP)为原料高选择性制备了一类Extended表面活性剂——壬基酚聚氧丙烯醚硫酸盐(NPPS)。探索了反应参数对选择性硫酸酯化的影响,优化后得到较佳的工艺条件为:n(HSO3Cl)/n(NPP)=1.3,老化温度35℃,老化时间15 min,此时硫酸酯化率达到98.4%,NPPS选择性达100%,且DMF钝化剂经简单回收后可重复使用。与非钝化氯磺酸法相比,该法实现了高选择性硫酸酯化;与氨基磺酸法相比,该法更简便、高效和廉价;因此,该法有望推广到其他同时含有醇羟基和芳香环原料的高选择性硫酸酯化反应中。
A method of highly selective sulfation of organic raw materials containing both alcoholic hydroxyl groups and aromatic rings was developed using DMF passivation of chlorosulfonic acid activity. Using this technology, nonylphenol polyoxypropylene ether (NPP) as a raw material for the highly selective preparation of an extended surfactant - nonylphenol polyoxypropylene ether sulfate (NPPS). The effects of reaction parameters on the selective sulfation were investigated. The optimum conditions were as follows: n (HSO3Cl) / n (NPP) = 1.3, aging temperature 35 ℃, aging time 15 min, The rate of 98.4%, NPPS selectivity of 100%, and DMF passivation agent can be reused after simple recovery. Compared with non-passivated chlorosulfonic acid method, the method achieves highly selective sulfation; compared with the sulfamic acid method, the method is simple, efficient and cheap; therefore, the method is expected to be extended to other alcohols containing both hydroxyl and Aromatic ring raw materials in the highly selective sulfation reaction.