Patent GB-342068-A (GB)
Title: A process for preparing concentrated nitric acid
Inventor: NIKODEM CARO
IPC: C01B21/46
Filed: 1929-12-06
Abstract: Nitric acid, particularly highly concentrated acid, is made by reacting oxygen or oxygen containing gases, water or aqueous nitric acid, and nitrogen oxides or liquid nitrogen tetroxide at temperatures above 70 DEG C., preferably 70 to 120 DEG C. and at pressures of 50 to 200 atmospheres or over.  The heating of the reactants and cooling of the acid produced is preferably carried out under full pressure whereby the reaction velocity is kept high.  The reaction mixture may first be heated to a high temperature to convert the greater part of the nitrogen tetroxide, the reaction being completed at decreasing temperature.  The reaction is carried out in pressure tubes, into which a gas mixture containing nitrogen oxides and oxygen under pressure is introduced from below, together with any liquid which may separate, and which may be mixed with water or aqueous nitric acid.  Alternatively, the gas mixture, after drying if necessary, may be cooled or treated with absorption agents to separate liquid nitrogen tetroxide. This is introduced into the pressure tubes with water or aqueous nitric acid, and compressed oxygen passed in.  The liquid initial materials may be sluiced in and a collecting chamber for the inflowing compressed gas provided, whereby large quantities may be used at the beginning, resulting in an instantaneous temperature rise, when no external heat is required. Heating or cooling jackets are provided if necessary.  The water and liquid nitrogen tetroxide may produce nitric acid before the pressure treatment, or nitric acid may be added.  The reaction may be carried out in stages, several pipes being united by gas and liquid conduits to provide different temperature and pressure stages.  Working may be intermittent or continuous.  To obtain pure, highly concentrated acid, the crude product is rectified at atmospheric air, or oxygen may be passed in, the gases removed being returned for recovery of nitrogen oxides.  The conduits, fittings and pressure chambers, or their linings, may be of alloys such as chromium steel.  Aluminium or its alloys is also suitable especially for the linings. Specification 116,495, [Class 1 (ii), Inorganic compounds, other than &c.], is referred to.  The Specification as open to inspection under Sect. 91 (3) (a) describes also the use of aluminium, pure, alloyed with other elements such as silicon, or coated with a protective layer or an oxide film, for building or lining apparatus for manufacturing highly concentrated nitric acid.  Aluminium linings at high pressures fit against the walls and support the pressure. Independent aluminium vessels may be placed in a pressure chamber, or intervals may be left and filled with neutral gas, or oxygen used in the nitric acid synthesis, so that equalization of pressure on the vessel is produced.  The aluminium envelope may be protected by a lining of ceramic material, such as quartz.  A little aluminium may be added to the liquid worked up, or the initial mixture may be prepared in aluminium apparatus, stored over rings of the same metal, or brought into contact with aluminium mud.  The pressure pipes may contain rings of the metal, or may be lined with aluminium, and the top and bottom closures may be similarly lined.  Connections for the acid and gas valves may extend through the covers, through which the compressed gas may be admitted e.g. by dipping devices.  The valves may be mounted on T-pieces.  The pipes may be packed or contain catalysts.  This subject-matter does not appear in the Specification as accepted, but forms the subject of a divided application.