| 摘要 |
1,153,971. Glycidol; glycerol. FMC CORP. 9 Jan., 1967 [11 Jan., 1966], No. 1108/67. Heading C2C. Glycidol is produced by epoxidation of allyl alcohol in the absence of water at 25-100‹ C. using a 15-40% by wt. solution of peracetic acid in an inert solvent, the ratio of allyl alcohol to peracetic acid being 5À0-0À7 mols alcohol per mol acid, and continuing epoxidation until at least 70% by wt. of the minor reactant has reached to convert allyl alcohol to glycidol in a yield of at least 90%. The glycidol recovered from the reaction mixture may be hydrolysed to glycerol at 25-170‹ C. using 10-100 mols water per mol glycidol. Specified solvents for the epoxidation are lower ketones, esters, ethers and alcohols, alone or in admixture with halogenated alkanes. Epoxidation is preferably effected at 25-100‹ C. using excess allyl alcohol and rapidly and continuously removing solvent and by-product acetic acid by distillation under reduced pressure, e.g., below 400 mm. Hg, and recovering glycidol which can be further purified and will yield a pure glycerol on hydrolysis. The process is illustrated by reference to flow sheet and apparatus drawings (not shown). |
