尿素反应耦合萃取分离处理乙炔清净工艺废硫酸的研究  

The treatment of spent sulfuric acid from the purification of acetylene by reacting with urea and coupling solvent extraction

作　　者：李娟 汪先富[2] 郭大林[2] 唐盛伟[1] 张涛[1] 

机构地区：[1]四川大学化学工程学院四川省多相流传质与反应工程重点实验室,四川成都610065 [2]四川天华富邦化工有限责任公司,四川泸州646207

出　　处：《应用化工》2017年第12期2378-2382,共5页Applied Chemical Industry

基　　金：国家自然科学基金项目(21576168);四川省科技支撑计划项目(2014GZ0058);川大-泸州战略合作项目(2014CDLZ-G29)

摘　　要：乙炔清净工艺产生的废硫酸酸度高且含有较多的有机杂质,有机杂质与硫酸分子能够形成强的相互作用处理困难。采用反应耦合萃取分离方法,利用尿素与硫酸分子形成硫酸脲,消除有机杂质与硫酸分子之间的作用力,同时耦合溶剂萃取可对反应后释放的有机杂质进行分离去除。研究了二氯甲烷/废硫酸体积比、反应时间、尿素/H_2SO_4摩尔比以及H_2SO_4浓度对废硫酸中有机碳去除率的影响。结果表明,二氯甲烷/废硫酸体积比和反应时间影响了有机杂质向萃取相的传质过程,尿素/H_2SO_4摩尔比和H_2SO_4浓度则对有机杂质的释放具有重要影响。较优的工艺条件为:二氯甲烷/废硫酸体积比3∶1,反应时间1.5 h;尿素/H_2SO_4摩尔比1.5∶1,H_2SO_4浓度64.56%。此时的有机碳去除率达到95.21%。The spent sulfuric acid( SSA) from the purification process of acetylene is difficult to deal with for the strong acidity and high content of organic impurities,the strong interaction between organic impurities and sulfuric acid was formed in SSA. The reaction coupling extraction separation method was adopted,and urea was used to react with sulfuric acid for the formation of urea sulfate in order to eliminate the interaction between organic impurities and sulfuric acid. Meanwhile,the released organic impurities could be separated by solvent extraction. The effects of the operation parameters including volume ratio of methylene chloride/SSA,reaction time,molar ratio of urea/H_2SO_4 and the H_2SO_4 concentration on the organic carbon removal ratio were investigated systematically. The results demonstrated that volume ratio of methylene chloride/SSA and reaction time affacted the mass transfer of organic impurities from SSA to extract phase,moreover,molar ratio of urea/H_2SO_4 and H_2SO_4 concentration have an important influence on the release of organic impurities. The organic carbon removal ratio could be obtained as 95. 21% under the optimal experimental conditions as follows: volume ratio of methylene chloride/SSA of 3∶ 1,reaction time of 1. 5 h,molar ratio of urea/H_2SO_4 of 1. 5∶ 1,H_2SO_4 concentration of 64. 56%.

关 键 词：废硫酸 反应耦合萃取法 有机碳去除率 硫酸脲 

分 类 号：TQ09[化学工程] TQ110.9