GB731438A - Improvements in or relating to manufacture of amyl nitrate - Google Patents

Abstract

A process for the nitration of amyl alcohols consisting essentially of between 80 to 100 per cent by weight of isomeric primary alcohols, of not more than 20 weight per cent isomeric secondary amyl alcohols and not more than 1 weight per cent tertiary amyl alcohol comprises reacting said amyl alcohols directly with a nitration mixture consisting essentially of nitric and sulphuric acids, the nitric acid in said mixture being at least 20 per cent by weight and the water in said mixture being not more than 14 per cent by weight, the amount of nitric acid in said mixture being at least equal to and not more than 13 per cent in excess of the stoichiometric requirement to substantially completely esterify said amyl alcohols, and the ratio by weight of water to sulphuric acid in the final esterification mixture being not more than 0.35. The process may be carried out batchwise or continuously. The reaction product is allowed to separate into two phases in a settling chamber or continuous centrifugation, and solvent extraction or distillation may be employed. The product is preferably washed with soda and percolated through a tower containing a solid adsorbent such as "Filtrol" (Registered Trade Mark) or silica gel. In examples a mixture consisting mainly of primary amyl alcohols with small amounts of secondary alcohols, diamyl ether and water and mixtures consisting of nitric acid, sulphuric acid and water are introduced into an agitated body of reaction liquid in a stainless steel vessel with an overflow leading to a series of separators, the second equipped with a line for the addition of soda ash solution. Various compositions of acid are employed and the feed ratio of acid to alcohol is varied p including both conditions in accordance with the invention and for comparison.