脂肪醇聚氧乙烯醚磺酸盐合成方法的改进  

SYNTHESIS OF FATTY ALCOHOL POLYOXYETHYLENE ETHER SULFONATES

作　　者：赵晓辉[1] 王云[1] 安东[1] 叶志文[1] 

机构地区：[1]南京理工大学化工学院,江苏南京210094

出　　处：《精细石油化工》2016年第1期11-16,共6页Speciality Petrochemicals

摘　　要：以脂肪醇、环氧乙烷、氯化亚砜和亚硫酸钾等为原料,依次通过阴离子聚合、氯代、磺化等反应合成了脂肪醇聚氧乙烯醚磺酸盐（AESO）。通过IR,13 C NMR,ESI-MS等手段对产物进行了结构表征。利用单因素法对各步反应的工艺条件进行了优化。各步反应的最佳条件为：阴离子聚合反应中,采用环氧乙烷间断式进样法,n（脂肪醇）∶n（环氧乙烷）=1∶4,催化剂氢氧化钠的用量为脂肪醇质量的0.1%,反应温度为115~125℃,反应压力为0.4 MPa,收率为44.2%;氯代反应中,以吡啶为催化剂,氯化亚砜为氯代剂,n（脂肪醇聚氧乙烯醚）∶n（氯化亚砜）∶n（吡啶）=1∶1.6∶0.8,70℃反应10h,收率为92.4%;磺化反应中,以水为溶剂,正己醇为稀释剂,质量均为氯代物质量的20%,亚硫酸钾为磺化剂,n（亚硫酸钾）∶n（氯代物）=1.5∶1,反应压力为1.0 MPa,155℃反应6h,经两相滴定法测得收率为91.3%。Fatty alcohol polyoxyethylene ether sulfonates was synthesized using fatty alcohols,ethylene oxide,thionyl chloride and potassium sulfite as raw materials in three steps including anionic polymerization,chlorination and sulfonation reaction.The target product was characterized by IR,13 C NMR and ESI-MS.The reaction conditions of each step were optimized through single factor experiment.The optimal conditions were confirmed depending on the experimental data：In anionic polymerization reaction,using intermittent injection of ethylene oxide,the molar ratio 1∶4（fatty alcohols：ethylene oxide）,the reaction temperature 115-125 ℃,pressure 0.4 MPa,the catalyst sodium hydroxide in an amount of 0.1% mass of fatty alcohols,yielding to 44.2%;In chlorination reaction,pyridine as the catalyst,thionyl chloride as the chlorinated agent,the molar ratio 1∶1.6∶0.8（alcohol polyoxyethylene ether∶thionyl chloride∶pyridine）,the reaction temperature 70 ℃,the reaction time 10 h,yielding to 92.4%;In sulfonation reaction,water as the solvent and n-hexanol as the diluent in an amount of 20% mass of halid,potassium sulfite as the sulfonating agent,the molar ratio1.5∶1（potassium sulfite：halid）,reaction temperature 155℃,pressure 1.0MPa,reaction time 6h,yielding to 91.3%.

关 键 词：脂肪醇聚氧乙烯醚磺酸盐 三次采油用表面活性剂 合成 

分 类 号：TQ423[化学工程]