双丙酮丙烯酰胺的合成

Synthesis of Diacetone Acrylamide

通过实验得出一步法合成DAAM(双丙酮丙烯酰胺)的最佳工艺条件是:物料配比:n_(丙酮):n_(丙烯腈):n_(硫酸)=2.4:1:1(物质的量之比,下同),反应最佳温度为65℃,反应时间为4h,精制后DAAM产率可达54.8％,纯度大于98％。两步法合成DAAM的最佳工艺条件是:在第一步双丙酮醇的合成中,丙酮回流时间10h;第二步DAAM的合成中最佳工艺条件同一步法。两步法合成DAAM的产率大于67％,纯度大于98％。在粗品精制过程中,无须减压蒸馏就可得到纯品。

The experimental results indicated an optimized one-stage process to prepare DAAM, with its formulation:n (acetone): n (acrylonitrile):n (sulfuric acid)=2.4:1:1,optimized reaction temperature: 65℃, reaction time:4 hrs.The refined DAAM gave a yield rate 54.8%, purity 98%. Two-stage process to prepare DAAM was optimized as: 10 h reflux time for acetone on the first-stage of diacetone alcohol synthesis. The second stage was controlled as the same as the first-stage. The refined DAAM by two-stage process gave a yield rate 67%, purity 98%. The raw intermediates can be refined to the final purified product without decompressed distillation during refining process.