文献类型：期刊文献

中文题名：络合法高效分离煤基粗酚中的间/对甲酚

英文题名：High efficient separation of m/p-cresols in coal-based crude phenols through complexing

作者：黄园园[1];周升[2];李永伦[2];张德祥[1]

机构：[1]华东理工大学能源化工系煤气化及能源化工教育部重点实验室,上海200237;[2]神华煤制油化工有限公司上海研究院,上海201108

年份：2016

卷号：45

期号：12

起止页码：1487

中文期刊名：石油化工

外文期刊名：Petrochemical Technology

收录：CSTPCD;;Scopus;北大核心:【北大核心2014】；CSCD:【CSCD2015_2016】；

基金：国家重点基础研究发展规划项目(2011CB201304)

语种：中文

中文关键词：煤基粗酚;间对甲酚分离;络合结晶法

外文关键词：coal-based crude phenols; separation of m/p-cresols; complexing and crystallization

摘要：在传统尿素络合法分离间/对甲酚的基础上,通过在络合反应过程中加入固体酸脱色剂以及使用混合溶剂对传统工艺进行改进。利用GC/MS、分光光度计等方法考察了固体酸脱色剂和溶剂对分离效果的影响,并采用正交实验获得最优工艺条件。表征结果显示,在络合反应中加入3%(w)的固体酸脱色剂可有效吸附产物中的含氮碱性化合物,产物脱色率达到94.35%。使用甲苯/正庚烷混合溶剂分离得到的间甲酚纯度和收率比使用甲苯溶剂高。实验结果表明,络合结晶分离间/对甲酚的最优条件为:间甲酚与尿素的摩尔比1∶1.2、结晶温度-15℃、溶剂与混酚体积比2∶1、甲苯与正庚烷的体积比1∶2、结晶时间120 min。在此条件下分离所得间甲酚的平均纯度和收率分别为99.43%和74.82%。将该工艺应用于煤基粗酚中间/对甲酚的分离提纯时,间甲酚纯度、收率和脱色率分别可达99.05%,72.33%,95.60%。
The traditional process for the separation of m/p-cresols in coal-based crude phenols through complexing and crystallization was improved by adding a solid acid decolorant and using mixed solvents. The influences of the solid acid decolorant and solvents on the separation process were investigated by means of GC/MS, spectrophotometer and orthogonal experiments. The results showed that, when the decolorant dosage was 3%（w） in the complex reaction, alkaline nitrogenous compounds in the products could effectively be adsorbed on the decolorant and the decolorization rate could reach 94.35%. Both the purity and yield of the m-cresol obtained by using the mixed solvents were higher than those obtained by using single toluene solvent. It was indicated that, under the optimized conditions of mole ratio of urea to m-cresol 1 ： 1.2, crystallization temperature -15 ℃, volume ratio of solvent to raw materials 2 ： 1, volume ratio of toluene to heptane 1 ： 2 and crystallization time 120 min, the average purity and yield of m-cresol could reach 99.43% and 74.82%, respectively. When this process was applied to the separation of the coal-based crude phenols, the purity, yield and decolorization rate of the m-cresol could reach 99.05%, 72.33% and 95.60%, respectively.