摘要
利用物性估算的方法估算了蒽、咔唑、二甲苯及氯苯间的范德华引力能,并测定了相应的溶解度.利用气质联用(GC-MS)对原料蒽渣中各个组分进行定性分析,以气相色谱内标标准曲线法对工艺过程中每一步所得产品中蒽、菲、咔唑和芴的含量进行了定量分析.结果表明,氯苯与蒽和咔唑间的引力能均大于二甲苯,与溶解度相一致.采用二甲苯两步溶解结晶后,菲和芴的去除率分别为96%和91%.以氯苯为溶剂精制咔唑,可得到含量为98.68%的高纯咔唑,咔唑的单程回收率在45%以上.
ABSTRACT Solvent selection is the key of solvent crystallization method. In this paper, based on the Matlab software, the intermolecular Van der Waal＇s attractive energy was calculat- ed between anthracene, carbazole, xylene and chlorobenzene molecules. GC-MS and GC with internal standard curve method were applied to determine the components of anthracene residue and content of anthracene, phenanthrene, carbazole and fluorene in the resulting products. The results showed that the intermolecular van der Waal＇s attractive energy between chlorobenzene and anthracene/carbazole was higher than that of xylene, which was consistent with the solubility data. After using xylene two steps of dissolution and crystallization, the removal efficiency of phenanthrene and fluorene was 96% and 91% respectively. DMF＋IPA co-solvent and chlorobenzene were applied to the process of anthracene and carbazole separation and carbazole refining, can get high purity carbazole with the purity of 98. 68%, the total recovery yield of carbazole is higher than 45 % without mother liquor recycling. KEY WORDS solvent crystallization method, anthracene residue, carbazole, property estimation
出处
《煤炭转化》
CAS
CSCD
北大核心
2013年第1期83-88,共6页
Coal Conversion
基金
太原市科技局项目(11014907)
高等学校博士学科点专项科研基金资助项目(20101402120009)
关键词
溶解结晶法
蒽渣
咔唑
物性估算
solvent crystallization method, anthracene residue, carbazole, property estimation
