四氟硼酸1-甲基-3-丁基咪唑盐的合成、表征及萃取脱硫探索

制备了环保型绿色离子液体——四氟硼酸1-甲基-3-丁基咪唑盐(BMIM]BF4),主要探讨"绿色合成"方法及其对模型油萃取脱硫的效果。在无溶剂条件下将N-甲基咪唑与1-氯代正丁烷通过高产率的亲核取代反应生成中间产物BMIM]Cl,再使其与NaBF4进行复分解反应生成目标物质,经红外光谱(FT-IR)、紫外光谱(UV)等测试方法验证可知,产物的分子结构为BMIM]BF4。考察了萃取时间、温度、含硫化合物种类(苯并噻吩BT或二苯并噻吩DBT)及剂油体积比对脱硫率的影响,在萃取温度40℃、萃取时间30min、剂油体积比1∶2的条件下,含DBT模型油的单级萃取脱硫率为54.4%。对含DBT模型油进行了三级萃取及离子液体回收再利用研究,结果表明,三级萃取脱硫率达到90%,离子液体可回收利用。

PREPARATION,CHARACTERIZATION AND EXTRACTIVE DESULFURIZATION PERFORMANCE OF 1-METHYL-3-BUTYL IMIDAZOLIUM TETRAFLUOROBORATE

An environment friendly ionic liquid (IL) 1-methyl-3-butyl imidazoliumtetrafluroborate (BMIM]BF4) was synthesized by green synthesis method. The investigations of preparation method and the extractive desulfurization performance were conducted. The intermediate product BMIM]Cl was obtained firstly by nucleophilic substitution reaction of N-methyl imidazolium and 1-chlorobutane under solvent-free condition, and then the product reacts with NaBF4 to get the target product (BMIM]BF4). The molecular structure was confirmed by characterization of UV、FT-IR、MS and13C-NMR. The effect of extraction time, extraction temperature, sulfur compound type (BT or DBT), ratio of IL to model oil on extractive desulfurization was presented. The multistage extraction of DBT model oil with IL BMIM] BF4 and its regeneration were studied. The results indicate that at the conditions of extraction temperature 40 ℃, 30min, and IL to oil volume ratio 1:2, the extraction desulfurization rate is 54.4% in single stage. While by 3 stage extractions, the sulfur removal rate is up to 90% and the IL can be recycled.