Process for the production and recovery of halonitroalkanes in high yield
AssigneeGreat Lakes Chemical Corporation
InventorsLarry D. Timberlake, James L. Brennan
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Abstract
A process for the preparation of halonitroalkanes, e.g. bromonitromethane, is disclosed in which a nitroalkane is reacted with an alkali metal base or an alkaline earth metal base, and the resulting nitroalkane salt is halogenated to form the halonitroalkane in a reaction mixture. The process is improved by acidifying the reaction mixture, preferably to pH=0-4, and thereafter recovering the halonitroalkane by azeotropic distillation of the reaction mixture. The acidification step increases the amount of halonitroalkane recovered, as compared to prior art processes in which the reaction mixture is distilled without prior acidification.
Claims12
In a method for the production and recovery of a halonitroalkane, the method including the preparation of the halonitroalkane in a reaction mixture at a final pH of at least about 5.0, the method further including the recovery of the halonitroalkane from the reaction mixture by azeotropic distillation, the improvement comprising:
- adjusting the pH of the reaction mixture to pH=0-4 prior to distillation recovery of the halonitroalkane, and thereafter recovering the halonitroalkane by azeotropic distillation.
A process for the preparation of a halonitroalkane which comprises the steps of:
- a. reacting a nitroalkane with an alkali metal base or an aIkaline earth metal base to form the nitroalkane salt;
- b. halogenating the nitroalkane salt produced by step a. to yield a reaction mixture including the halonitroalkane and having a pH of at least about 5;
- c. reducing the pH of the reaction mixture of step b. to pH=0-4;
- and
- d. after step c., recovering the halonitroalkane by azeotropic distillation of the pH-adjusted reaction mixture.
A process for the preparation of a halonitroalkane which comprises the steps of:
- a. reacting a nitroalkane with an alkali metal base or an alkaline earth metal base to form the nitroalkane salt;
- b. halogenating the nitroalkane salt produced by step a. to yield a reaction mixture including the halonitroalkane;
- c. reducing the pH of the reaction mixture of step b. by at least about 1;
- and
- d. after step c., recovering the halonitroalkane by azeotropic distillation of the pH-adjusted reaction mixture.
Dependencies are inferred from the claim text.