摘要
以季戊四醇、三氯化磷和双酚A作为原料合成了抗氧剂二亚磷酸二(双酚A)季戊四醇酯.探索了物料配比、反应溶剂的种类及用量和反应时间等反应条件对产率的影响,并通过正交试验法确定了适宜工艺条件.试验结果表明:反应溶剂为苯,用量为50 mL;物料配比[m(季戊四醇):m(三氯化磷):m(双酚A)]为1.0:2.8:2.0;第一步和第二步均回流反应3 h.在适宜工艺条件下所制得的产品为白色粉末状固体,熔点为146℃~148℃,产率约为93%.此外,通过元素分析、红外谱图和核磁共振对产品进行了物性和结构表征.
Dibiphenol A pentaerythritol diphosphite was synthesized by using pentaerythritol, phosphorus trichloride and hisphenol A as raw material. The effects of reaction solvent, reaction time and molar ratio of the raw material on yields were analyzed. The experimental results show that the optimum conditions were as follows:molar ratio of pentaerythritol to phosphorus trichloride to hisphenol A was 1.0:2.8:2.0, the first and the second reaction held for about 3 h on the conditions of refluxing. The product, under this conditions, was awhite flour solid and the melting point was 146 ℃--148℃, the yield of the product was about 93%. Elemental analysis, IR, and ^1 HNMR were performed to characterize the structure of the product.
出处
《化学工业与工程》
CAS
2005年第6期434-437,共4页
Chemical Industry and Engineering