高纯度2-羟基对苯二甲酸的合成新技术

化工进展

高纯度2-羟基对苯二甲酸的合成新技术

金宁人1，谢品赞1，张建庭1，孙刚1，胡燕红2，赵德明1

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

出版日期:2011-08-05 发布日期:2011-08-05

Synthesis of high-purity 2-hydroxyterephthalic acid

JIN Ningren1，XIE Pinzan1，ZHANG Jianting1，SUN Gang1，HU Yanhong 2，ZHAO Deming1

1College of Chemical Engineering and Materials Science，Zhejiang University of Technology，Hangzhou 310032，Zhejiang，China；2 Dragon Chemicals Group Company，Hangzhou 310005，Zhejiang，China

Online:2011-08-05 Published:2011-08-05

摘要/Abstract

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。

Abstract:

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 CO₂atmospheric 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.

金宁人1，谢品赞1，张建庭1，孙刚1，胡燕红2，赵德明1. 高纯度2-羟基对苯二甲酸的合成新技术 [J]. 化工进展.

JIN Ningren1，XIE Pinzan1，ZHANG Jianting1，SUN Gang1，HU Yanhong 2，ZHAO Deming1. Synthesis of high-purity 2-hydroxyterephthalic acid[J]. Chemical Industry and Engineering Progree.