【摘要】 研究了以3,5-二叔丁基-4-羟基-苯甲酸和2,4-二叔丁基苯酚为原料,SOCl2为酰化试剂,一锅法合成光稳定剂3,5-二叔丁基-4-羟基-苯甲酸-2,4-二叔丁基苯基酯的工艺.通过实验考察了投料比、温度及酰化试剂用量对反应的影响,确定了较佳的工艺条件:3,5-二叔丁基-4-羟基-苯甲酸与2,4-二叔丁基苯酚的物质的量比为1∶1.1;酰化剂SOCl2与3,5-二叔丁基-4-羟基-苯甲酸的物质的量比为1.2∶1;反应温度为70℃;反应时间为11 h.还考察了结晶溶剂的种类、用量和温度对产品质量和收率的影响,得到了较佳的结晶工艺条件:V(正丁醇)/m(初产物)为1.4 m L/g;结晶温度为25℃.产品总收率可达83.0%.更多还原

【Abstract】 The novel process preparation of the light stabilizer 2,4-di-tert-butylphenyl 3,5-di-tert-butyl-4-hydroxybenzoate by one-pot reaction was studied. The synthesis used 3,5-di-tert-butyl-4-hydroxy-benzoic acid and 2,4-di-t-butylphenol as raw material and SOCl2 as acylation reagent. The effects of raw ratio,temperature and catalyst dosage on the reaction were investigated. The optimum reaction conditions were selected as follows: the molar ratio of 3,5-di-tert-butyl-4-hydroxy-benzoic acid to 2,4-di-t-butylphenol was 1 ∶ 1. 1,the molar ratio of SOCl2 to 3,5-di-tert-butyl-4-hydroxy-benzoic acid was 1. 2 ∶ 1; the reaction temperature was 70 ℃;the reaction time was 11 hours. The effects of solvent kind,dosage and temperature on the product quality and crystallization yield were also investigated. The optimum conditions showed that: the ratio of 1-butanol and crude product was 1. 4 mL / g,the temperature of crystallization was 25 ℃. The total yield reached 83. 0%.更多还原