2,8-二甲基壬二酸的合成及其电化学性能研究  

SYNTHESIS AND ELECTRONIC CHEMICAL PERFORMANCE OF 2,8-DIMETHYL AZELAIC ACID

作　　者：刘长春[1] 闻立新[1] 刘承先[1] Liu Changchun;Wen Lixin;Liu Chengxian(College of Chemistry and Materials Engineering,Changzhou Institute of Engineering and Technology,Changzhou 213164,Jiangsu,China)

机构地区：[1]常州工程职业技术学院化学与材料工程学院,江苏常州213164

出　　处：《精细石油化工》2018年第4期53-57,共5页Speciality Petrochemicals

基　　金：江苏高校品牌专业建设工程资助项目(项目编号PPZY2015B178);江苏省高校优秀中青年教师和校长境外研修计划资助

摘　　要：以2,8-壬二酮和α-溴代乙酸乙酯为原料,经Darzens缩合、皂化、酸析、脱羧及氧化反应制备得2,8-二甲基壬二酸,总收率80.8%(以2,8-壬二酮计),通过~1H NMR、^(13)C NMR、IR和元素分析对所有产物结构进行了表征。考察了原料配比、反应温度和反应时间对Darzens缩合反应的影响,反应温度和臭氧流量对臭氧氧化反应的影响。结果表明,较佳的反应条件为:Darzens缩合反应,n(2,8-壬二酮)∶n(α-溴代乙酸乙酯)∶n(乙醇钠)=1∶2.5∶2.5、80℃回流反应8h;臭氧氧化反应,反应温度30℃、臭氧流量600mL/min。用该2,8-二甲基壬二酸在乙二醇中与氨气反应制备的电解质溶液,电导率达2.98mS/cm,闪火电压432V,氧化效率可达2.01(2mA),测试性能优于现有市售产品。2,8-Dimethyl azelaic acid was synthesized by using 2,8-nonanedione andα-bromoacetate via Darzens condensation,saponification,acidification and oxidation reactions with the total yield of 80.8%（based on 2,8-nonanedione）.All products＇ structures were characterized by 1H NMR,（13）C NMR,IR and elemental analysis.The effects of raw material ratio,reaction time and reaction temperature on Darzens condensation reaction,the effects of reaction temperature and ozone flow rate on ozonation were investigated.The result shows that the optimized process is：in Darzens condensation reaction,the molar ratio of 2,8-nonanedione,α-bromoacetate and sodium ethoxide is 1∶2.5∶2.5,reaction tempature is 90 ℃（reflux）,reaction time is 8 h;in ozonation reaction,reaction tempature is 30℃,ozone flow rate is 600 mL/min.After reacting with ammonia,2,8-dimethyl azelaic acid was used to prepare an electrolyte with the conductivity of 2.98 mS/cm,the spark voltage of 432 V,and a high oxidizing efficiency of 2.01（2mA）,which performance was superior to commercially available products.

关 键 词：2 8-二甲基壬二酸 高压铝电解电容器 电解液 Darzens缩合 臭氧氧化反应 闪火电压 

分 类 号：O623.6[理学—有机化学]