煤气化粗酚中低级酚的分离研究  

Study on separation of low-carbon phenols from coal gasification by-products

作　　者：李焕新[1] 梁淑琴[1] 张丹[1] 李惠萍[1] 

机构地区：[1]郑州大学化工与能源学院,河南郑州450001

出　　处：《现代化工》2016年第10期150-153,共4页Modern Chemical Industry

摘　　要：针对煤气化粗酚组成特点设计并搭建了粗酚预处理装置（1^#塔）和苯酚与甲酚分离装置（2^#塔）,同时进行了物料衡算。实验考察了回流比R对产品质量的影响。结果表明,当R=5～7时,可回收约75%、质量分数高达99.8%的苯酚;当R=9^10时,获得甲酚质量分数87%的产品,回收率约为57%。然后以甲酚为原料,采用单因素实验考察了主要工艺参数对尿素络合法分离3-甲基苯酚的质量分数及回收率的影响。结果表明,在n（尿素）∶n（3-甲基苯酚）=1.43∶1,V（溶剂）∶V（混酚）=3.5∶1,络合反应温度为90℃,反应时间60 min和终止析出温度为-15℃,结晶时间100 min条件下,3-甲基苯酚回收率约为55%,质量分数达97%以上。最后,采用溴化钙络合法调节尿素络合法获得的滤液中3-甲基苯酚和4-甲基苯酚的比例2∶1,以循环采用尿素络合法提高3-甲基苯酚的回收率。结果显示,当n（Ca Br2）∶n（4-甲基苯酚）=0.6∶1,反应6 h时,最终可使3-甲基苯酚的总回收率提高至70%。The pretreater（ the 1~#tower） and the separation tower for phenol and cresols（ the 2~#tower） are designed and built on the basis of the composition characteristics of crude phenols. The material balance is carried out.The influence of the reflux ratio（ R） on the quality of the products is studied. The results show that when R = 5- 7,the recovery of phenol is about 75% but the purity is as high as 99. 8%. When R = 9- 10,the content of cresols is 87%,and the recovery is about 57%. Then using the cresols as raw material,the influence of the main process parameters on the purity and recovery of 3-methyl phenol are studied with urea complex method by using the single factor experiment. The recovery of 3-methyl phenol is 55% and the purity is above 97% under the following conditions： 1. 43∶ 1. 0 of the molar ratio of urea to 3-methyl phenol,3. 5∶ 1. 0 of the volume ratio of solvent to 3-methyl phenol,90℃ of the complex reaction temperature,60 minutes of reaction time and- 15℃ of the termination of the precipitation temperature. Finally,the calcium bromide（ Ca Br2） is used as complexing agent and reacts with 4-methyl phenol to adjust the ratio of 3-methyl phenol to 4-methyl phenol in the filtrate from the process of the urea complex method to 2 ∶ 1. When the molar ratio of Ca Br2 to 4-methyl phenol is 0. 6,the reaction time is above 6 hours,the content of 3-methyl phenol in the filtrate can be increased up to 50%. The total recovery rate can be up to 70%.

关 键 词：煤气化粗酚 苯酚 3-甲基苯酚 分离 

分 类 号：TQ243.12[化学工程—有机化工]