2,6-二异丙基萘液相氧化制备2,6-萘二甲酸工艺条件的研究  

STUDY ON THE CATALYTIC OXIDATION PROCESS OF PREPARING 2,6-NAPHTHALENEDICARBOXYLIC ACID FROM 2,6-DIISOPROPYLNAPHTHALENE IN LIQUID PHASE

作　　者：李达仁[1,2] 靳海波[1] 史高峰[2] 

机构地区：[1]北京石油化工学院化工系,北京102600 [2]兰州理工大学石油化工学院

出　　处：《石油炼制与化工》2006年第6期14-17,共4页Petroleum Processing and Petrochemicals

基　　金：中国石化股份有限公司科技开发部资助项目(编号:201069)。

摘　　要：以乙酸钴、乙酸锰为主催化剂，溴化钾为促进剂，乙酸钾为助催化剂，在半连续搅拌钛材釜式反应器中，对2，6-二异丙基萘（2，6-DIPN）液相空气氧化制2，6-萘二甲酸的主要氧化工艺条件进行了研究。采用高效液相色谱内标法分析2，6-萘二甲酸的纯度和收率，考察了反应时间、M／F、混合溶剂、催化液循环使用次数对氧化反应的影响，从而确定半连续反应合适的工艺条件为：反应时间4～5h，M／F=1.2～1.6，V（丙酸）／g（醋酸）-0．5～0．7。M／F=2．4时催化液可多次循化使用。在温度200℃，压力3．0MPa，搅拌速度900r／min，V（丙酸）／V（醋酸）-0．5，M／F=1.2，n（Co）：n（Mn）：n（Br）：n（K）=1：1：2：5的条件下反应4h，2，6-萘二甲酸的收率和纯度分别可达82．76％和98．56％。The process conditions of preparing 2,6-naphthalenedicarboxylic acid（2,6-NDCA） by air-oxidizing 2,6-diisopropylnaphthalene（2,6-DIPN）in liquid-phase were studied in a semi-continued titanium reactor with stirring, using cobalt acetate and manganese acetate as main catalyst, potassium bromide as promoter,potassium acetate as co-catalyst. Inner standard method of HPLC was applied to analyze the purity and yield of 2,6-NDCA. The effects of reaction time,tool ratio of metal catalysts to 2, 6-DIPN（M/F） ,type of solvents and catalyst recycle times on the oxidation reactions were investigated. The optimum reaction conditions were obtained, which was a reaction time range of 4～5 h,M/F mol ratio range of 1.24 1.6, and using propionate acid and acetic acid（volume ratio range of 0.5～0.7）as mixed-solvent. When the oxidation process was proceeded at a reaction temperature of 200℃ ,a reaction pressure of 3.0 MPa,a reaction time of 4 h,a M/F ratio of 1.2,using mixed-solvent with a mixing ratio of 0.5,and the catalyst having metal ratios of n（Co） ： n（Mn） ： n（Br） ： n（K）=1 ： 1 ： 2 ：5,the yield and the purity of the 2,6-NDCA obtained were 82.76% and 98.56% ,respectively.

关 键 词：2 6-二异丙基萘 2 6-萘二甲酸 氧化过程 操作条件 

分 类 号：TQ245.12[化学工程—有机化工]