论文部分内容阅读
依据量子化学理论计算 ,设计并优化了 1-苯基二苯并膦 (1- phenydibenzophosphole,简称 PDBP)磺化制备二磺化 1-苯基二苯并膦 (5 H- phenyl- 3,13- disulfonatodibenophosphole,简称 PDBPDS)的工艺 ,重点探讨了 SO3/PDBP比、反应温度、反应时间以及硼膦比对磺化产物收率的影响 .实验结果表明 ,采用 5 0 %发烟硫酸作磺化剂、SO3/ PDBP摩尔比为 3,H3BO3/ PDBP比为 5 ,在 13～ 15℃及无水无氧条件下反应 5 0 h,磺化产物收率可达 85 % .此外 ,还将所得产物用作丙烯氢甲酰化两相反应催化剂的配体 ,大大提高了催化剂的活性和产物正异比 ,且有机相中铑含量仅为 3.6× 10 - 8,有效地控制了铑流失 .实验结果证明了新型水溶性配体 PDBPDS是一个能实现均相反应多相化的、很有开发前景的配体 .
Based on the quantum chemistry theory, the sulfonation of 1-phenyldibenzophosphole (PDBP) was designed and optimized to prepare 5-phenyl-3, disulfonatodibenophosphole (abbreviated as PDBPDS), the effects of SO3 / PDBP ratio, reaction temperature and reaction time on the yield of sulfonated products were discussed.The results showed that using 50% oleum as sulfonating agent, SO3 / PDBP molar ratio of 3, H3BO3 / PDBP ratio of 5, the reaction of 5h at 13 ~ 15 ℃ and anhydrous anaerobic conditions, the yield of sulfonated products can reach 85% .In addition, Propylene hydroformylation of the two - phase catalyst ligand greatly enhances the activity of the catalyst and the product of different ratio, and the organic phase rhodium content of only 3.6 × 10 - 8, effectively control the rhodium loss.Experimental results show that The new water-soluble ligand PDBPDS is a well-developed ligand that can achieve homogeneous reaction heterogeneity.