【摘要】 以甲醛、异丁醛和季戊四醇为主要原料,在催化剂作用下利用循环一锅法合成螺二醇。通过正交优化实验,考察了物料配比、温度、反应时间、溶剂量以及催化剂对两步法合成螺二醇收率的影响,确定了合成螺二醇最佳工艺条件,在该适宜条件下,开发了循环一锅法的制备工艺,即n(甲醛):n(异丁醛):n(季戊四醇)=2.85:2.85:1,反应温度75℃,反应时间9 h,产品总收率和纯度可达95.4%和99.9%。采用~1HNMR和HPLC确定了螺二醇产品结构和纯度。更多还原

【Abstract】 Spiroglycol is synthesized by circulating one-pot method with formaldehyde,isobutylaldehyde and pentaerythritol as main materials under catalysts.Based on the orthogonal tests,the factors influencing the yield of spiroglycol,such as molar ratio of reactants,reaction temperature,reaction time,the dosage of catalysts and solvent,are investigated for two-step meth- od,and the optimal reaction conditions are obtained.Under the optimal conditions,the circulating one-pot method for prepar- ing spiroglycol is studied.The total yield reaches to 95.4% and the purity reaches to 99.9% when the molar ratio of formalde- hyde to isobutylaldehyde and pentaerythritol is 2.85:2.85:1,the reaction time is 9 h,the reaction temperature is 75℃.The structure and purity of spiroglycol are determined by ~1HNMR and HPLC.更多还原