摘要
采用溶剂法以对苯二酚和氢氧化钾为原料,在高压二氧化碳条件下合成了2,5-二羟基对苯二甲酸,考察了反应压力、溶剂、搅拌速率及氢氧化钾用量对收率的影响,用高效液相法分析了产物的纯度,用元素分析、FT-IR、~1H NMR和^(13)C NMR方法表征了产物结构。较佳合成条件为:以正辛烷为溶剂,反应温度220℃,m (对苯二酚):m(KOH)=2．75:7,反应压力11．5MPa,搅拌速率400r/min,反应时间4h。在此条件下,2, 5-二羟基对苯二甲酸的收率为76．52%。
2,5-Dihydroxyterephthalic acid was prepared from hydroquinone and potassium hydroxide. The effects of the reaction pressure, solvent, stirring rate and the amounts of KOH and K2CO3 on the yield of 2,5-dihydroxyterephthalic acid were examined. The purity of the product was analyzed by HPLC and the structure of product was characterized by elementary analysis, FT-IR, ^1H NMR and 13C NMR. Under the following conditions： hydroquinone to KOH weight ratio 13.75 ： 35, 150 mL noctane as solvent, reaction temperature 220 ℃, reaction pressure 11.5 MPa and stirring rate 400 r/ min, the yield of 2,5-dihydroxyterephthalic acid was up to 76.52 % after reaction for 4 h.
出处
《精细石油化工》
CAS
CSCD
北大核心
2007年第1期23-25,共3页
Speciality Petrochemicals
关键词
2
5-二羟基对苯二甲酸
合成
表征
溶剂法
2,5-dihydroxyterephthalic acid
synthesis
characterization
solvent method
