摘要
以季戊四醇、三氯化磷和2,4-二叔丁基苯酚为原料,在实验室合成了双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯。采用正交试验考察了反应温度、反应时间、催化剂及物料配比对产品收率的影响。试验结果表明,整个工艺过程适宜的工艺条件为:2,4-二叔丁基苯酚、三氯化磷和季戊四醇的摩尔比为2.00∶2.05∶1.00,催化剂B的用量为季戊四醇质量的2.2%,第一步反应温度为130℃,时间为2.5 h;第二步反应温度为120℃,时间3.0 h。产品元素分析及红外光谱与目的产物相一致。
Bis(2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphitc (antioxidant 626) was synthesized with pentaerythritol, di-tert-butylphenol and phosphorus trichloride. The effects of reaction temperature, reaction time, catalyst and the molar ratio of raw materials on the yield of the product were discussed by orthogonal experiment. From the experimental results, the optimized conditions were obtained. The first reaction was carried out at 55 ℃ for 3 h, while the second reaction at 125 ℃ for 2 h. The molar ratio of pentaerythritol, phosphorus trichloride and di-tert-butylphenol is 1 : 2.05 : 2.0, and the weight ratio of catalyst B to pentaerythritol is 0.022. The element analysis and IR spectrogram of the product agreed well with the target product.
出处
《化学工业与工程》
CAS
2008年第4期319-323,共5页
Chemical Industry and Engineering