二亚磷酸二(2,6-二叔丁基对甲酚)季戊四醇酯的合成

Synthesis of Di(2,6-di-tert-butyl-p-cresol) Pentaerythritol Diphosphite

以亚磷酸三乙酯、季戊四醇和2,6-二叔丁基对甲酚为原料合成了抗氧剂二亚磷酸二（2,6-二叔丁基对甲酚）季戊四醇酯。探讨了物料配比、催化剂的种类及用量、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最佳工艺条件。实验结果表明：催化剂为无水碳酸钾,其用量为0.6 g;物料配比（n（季戊四醇）∶n（亚磷酸三乙酯）∶n（2,6-二叔丁基苯酚））为1.0∶2.12∶2.04;反应Ⅰ温度为130~140℃,反应Ⅰ时间为2 h,反应Ⅱ温度为170~180℃,反应Ⅱ时间为4 h。在最佳工艺条件下所制得的产品为白色粉末状固体,熔点为67~69℃,产率为87%左右。此外,通过元素分析、红外光谱分析对产品进行了物性和结构表征。

Di（2,6-di-tert-butyl-p-cresol） pentaerythritol diphosphite was synthesized by using pentaerythritol,triethyl phosphate and 2,6-di-tert-butyl-p-cresol as raw materials.The effects of reaction solvent,reaction time and molar ratio of raw materials on yields were analyzed,and the optimum technological conditions were determined according to orthogonal experiments.The experimental results show that the optimum conditions were as follows： the n（pentaerythritol）： n（triethyl phosphate）： n（2,6-di-tert-butyl-p-cresol） molar ratio is 1.0∶2.12∶2.04,for reaction I the reaction temperature is ranged from 130℃ to 140℃ and the reaction time is 2h,for reaction II the reaction temperature is ranged from 170℃ to 180℃ and the reaction time is 4h.The product,obtained under the optimum conditions,was white flour solid and its melting point was 67～69℃,the yield of the production was about 87%.Elemental analysis,IR were also performed to characterize the structure of the product.