PROCEDIMIENTO CONTINUO DE EXTRACCIËN DE BROMO, DIRECTAMENTE EN ESTADO LIQUIDO, A PARTIR DE UNA SOLUCIËN DE ACIDO BROMOSULFURICO

摘要

Bromine is prepared from hydrobromic acid or mixtures containing it by oxidation with nitric acid or nitrogen oxides, such as those obtained by the combustion of ammonia, in a solution of acidity at least 5N. The hydrobromic acid-containing mixture may be that obtained in the recovery of bromine from sea water by treatment of brominated air with sulphur dioxide and spray water and consists of a mixture of HBr and H2SO4, referred to in the Specification as "bromosulphuric acid." Bromo-sulphuric acid containing 50-250 g. HBr per litre is fed via line 1 (see drawing) to packed column 2 and thence to reaction zone 3 supplied with nitric acid, e.g. 50-70% concentration, through line 4 and make-up mineral acid to achieve the required acidity through line 5. The reaction solution is maintained, preferably under atmospheric pressure, at between room temperature and the boiling point of bromine by inserting cooling means between reactor 3 and column 2, or the bromosulphuric acid may be pre-cooled to below room temperature. When the bromosulphuric acid concentration is 70-100 g. per litre, or the make-up acid is sulphuric acid of low concentration, or is hydrochloric acid, heat is required to promote the reaction. Sulphuric acid in the reaction solution is preferably 20 to 36% by weight. Bromine formed flows through line 7 to packed column 8 maintained at near room temperature and air or oxygen entering via 9 carries away entrained nitrosyl bromide via pipe 10 to the bottom of column 2. The bulk of the NoBr produced in reactor 3, plus that arriving via pipe 10, plus air or oxygen introduced via line 6, ascends column 2 and, in contact with descending bromosulphuric acid, is converted to nitric and hydrobromic acids which return to the reactor 3. Residual acid from reactor 3 passes via line 12 to packed column 13 into which steam and optionally air or other inert gas is passed via line 14. Dissolved bromine is thereby returned to reactor 3 via line 15. Bromine-free residual acid leaves via line 16, gases via 17 and bromine via line 11.