摘要
以对苯二酚、碳酸氢钾和碳酸钾为原料,在少量溶剂条件下,合成2,5-二羟基对苯二甲酸。考察了反应温度、反应压力、反应时间对收率的影响。用高效液相色谱法分析产物的纯度,用DSC测定产物熔点、^(1)H NMR确定产物结构。得出最佳合成条件为m(对苯二酚)∶m(碳酸氢钾)∶碳酸钾=3∶10∶1,反应温度220℃,反应压力2.0~2.5MPa,反应时间12h左右。在此条件下,2,5-二羟基对苯二甲酸的收率为65.5%。
The 2,5-dihydroxyterephthalic acid is prepared with the hydroquinone,potassium bicarbonate and potassium carbonate as the raw materials and small amount of solvent.The effects of reaction temperature,reaction pressure and reaction time on the yield of 2,5-dihydroxyterephthalic acid are investigated.The purity of the product is analyzed by HPLC,the melting point of the product is determined by DSC and the structure of product is confirmed by ^(1)H NMR.Under the following conditions:the weight ratio of hydroquinone to KHCO3 to K2 CO3 is 3∶10∶1,the reaction temperature is 220℃,the reaction pressure is 2.0~2.5 MPa and the reaction time is 12 h,the yield of 2,5-dihydroxyterephthalic acid reaches 65.5%.
作者
曹龙海
于振
王文彬
CAO Long-hai;YU Zhen;WANG Wen-bin(Institute of Petrochemistry,Heilongjiang Academy of Sciences,Harbin 150040,China)
出处
《化学与粘合》
CAS
2021年第6期432-434,共3页
Chemistry and Adhesion
基金
黑龙江省科学院科学研究基金项目(编号:ZS_(2)019002)。
关键词
2
5-二羟基对苯二甲酸
放大
工艺
研究
2,5-Dihydroxyterephthalic acid(DHTA)
scale-up
process
study
