高纯度2-羟基对苯二甲酸的合成新技术  

Synthesis of high-purity 2-hydroxyterephthalic acid

作　　者：金宁人[1] 谢品赞[1] 张建庭[1] 孙刚[1] 胡燕红 赵德明[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310032 [2]鼎龙化工集团公司,浙江杭州310005

出　　处：《化工进展》2011年第8期1789-1794,1814,共7页Chemical Industry and Engineering Progress

基　　金：江苏省科技攻关重大项目(BE2006077)

摘　　要：系统地研究了以间羟基苯甲酸(HBA)为原料、经改进的Koble-Schmitt法常压合成2-羟基对苯二甲酸(HTA)的新工艺及其精制方法,并与2-溴对苯二甲酸(BTA)催化水解法制备HTA技术进行了比较。结果表明:以HBA为原料,甲酸钾为溶剂,在碳酸钾存在下,反应温度为230～240℃时,CO2常压羧化反应6 h制得纯度约90%的HTA粗品,采用二次酸碱精制法可使HTA质量达聚合级单体的水平(纯度>99.5%,金属离子<50 mg/kg),总收率56%以上。产品经FT-IR和MS表征确认。该技术具有常压反应、操作方便、产品质量优异、经济性良好及易于产业化等优点,能为进一步合成羟基改性的新型高性能材料及新单体提供原料。2-hydroxyterephthalic acid（HTA）was synthesized by modified Koble-Schmitt atmospheric carboxylation method.and refined.The new synthesis method was compared with 2-bromoterephthalic acid（BTA）catalytic hydrolysis.The results showed that crude product HTA with purity of 90% was prepared from HBA by CO2 atmospheric carboxylation for 6 h at 230—240 ℃ in the presence of K2CO3 and potassium formate solvent,and purified through two times acid-alkali refining to obtain polymerization-grade HTA with high-purity of 99.5 % and metal ions of below 50 mg/kg,total yield of above 56%（base on HBA）.The prepared HTA was identified by FT-IR and MS,and the process had the advantages of atmospheric carboxylation,convenient operation,excellent product quality,good economy and easy commercialization.The prepared HTA could provide the raw material for new high-preformance materials modified with hydroxy group and new monomers.

关 键 词：2-羟基对苯二甲酸 甲酸钾 改进的Koble-Schmitt法 常压羧化 间羟基苯甲酸 

分 类 号：TQ246.3[化学工程—有机化工]