Patent GB-806732-A (GB)
Title: Preparation of compounds of uranium and non-metals
IPC: C01G43/00
Filed: 1946-02-15
Abstract: Uranium compounds of non-metallic elements particularly fluorine, iodine, bromine, chlorine, sulphur, selenium, tellurium, nitrogen, phosphorus, arsenic, antimony, carbon and boron are prepared by reacting uranium hydride with the non-metallic elements or compounds thereof.  The uranium hydride may be prepared by reacting uranium with hydrogen which is preferably obtained by the decomposition of previously prepared uranium hydride.  The non-metal component may be reacted as such if it is easily volatilizable but otherwise should preferably be converted into a volatilizable compound before reaction.  Preferably hydrides of the non-metal are reacted, for example ethane, ethylene, butylene, acetylene, hydrohalides such as hydrogen chloride, hydrogen fluoride, hydrogen iodide or hydrogen bromide, borohydrides such as diborane, phosphorus hydride, silicon hydrides, hydrogen telluride, arsenic hydride, hydrogen sulphide, hydrogen selenide or ammonia.  Oxides such as sulphur dioxide or trioxide, nitrogen oxides such as nitric and nitrous oxide, phosphorus trioxide, chlorine monoxide, chlorine dioxide, and carbon monoxide and dioxide may also be reacted.  By reaction of such oxides, compounds of uranium, the non-metal and oxygen such as uranium sulphate or phosphate may be prepared.  In addition two non-metals such as carbon tetrachloride, carbon tetrabromide, silicon tetrachloride, carbon tetrafluoride, boron trifluoride or carbon disulphide may be used to produce compounds of uranium and one or both of the non-metals depending on the molar proportions present. The uranium hydride is preferably prepared in situ in the reactor by reacting uranium with hydrogen at 200-400 DEG  C. Prior to the hydrogen treatment the uranium metal may be cleaned with an acid, such as 6 normal nitric acid.  The hydride so formed may be reacted with the non-metal or its compound in the gaseous or dissolved state, at temperatures ranging generally between 200-600 DEG  C.  According to examples: (1) uranium metal was heated to 250 DEG  C. in a copper reaction vessel and reacted with hydrogen. After the hydried was formed, hydrofluoric acid was introduced in a slow stream and the reactor maintained at 250 DEG  C., thereby converting the hydride into uranium tetrafluoride.  (3) Uranium hydride was reacted with hydrochloric acid gas at 250 DEG  C. to produce uranium trichloride. Uranium tribromide, tetraiodide or dioxide may be similarly prepared employing hydrobromic acid, hydroiodic acid or steam.  (6) Uranium hydride prepared as above was reacted with gaseous hydrogen sulphide at 500 DEG  C. to produce uranium disulphide.  (7) Uranium hydride was reacted with phosphine at 400 DEG  C. to produce a greyish-black phosphide of formula U2P3.  Uranium carbide may be prepared by reacting ethylene in lieu of phosphine at about 500 DEG  C.  (9) Carbon tetrachloride vapour was passed over uranium hydride, the reaction occurring rapidly at 500 DEG  C. with a production of UCl4 which was distilled out of the reaction mixture.  (10) Hydrogen was bubbled through methyl iodide at room temperature and the methyl iodide saturated hydrogen was passed over uranium hydride at 300 DEG C. to produce uranium triodide.  (11) Phosgene was passed over uranium hydride powder in a horizontal tubular reaction chamber at 150 DEG  C. to produce uranium tetrachloride contaminated with some carbon.  (12) Chlorine diluted with argon in a proportion of 1-9 was passed over uranium hydride at room temperature, the reaction proceeding smoothly to produce uranium tetrachloride which was distilled from the reaction mixture after reaction was completed. Specification 806,731 is referred to.