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United States Patent Office Patented Aug 3,830,906 United States Patent Office Patented Aug. 20, 1974 to decompose thermally. This order of operations is high- 3,830,906 ly desirable if high yield and purity are to be obtained. TWO STEP PROCESS FOR PRODUCING The process of the present invention exhibits a number BERYLLIUM HYDRIDE FROM A BERYL- of distinct advantages over previously known methods for HUM HALIDE g the preparation of beryllium hydride. Previous methods Roy J. Laran, Greenwell Springs, and Paul Kobetz, required the separation of beryllium alkyl from a reaction Baton Rouge, La., and Robert W. Johnson, Jr., mixture containing, in addition, aluminum chloride or ex- Savannah, Ga., assignors to Ethyl Corporation, New cess aluminum alkyl. Since both aluminum and beryllium York, N.Y. alkyls are highly reactive and flammable in air, the sep- No Drawing. Filed Apr. 23, 1965, Ser. No. 451,694 Int. CI. COlb 6/00 10 aration of the beryllium alkyl from the reaction mixture U.S. CI. 423—645 8 Claims and its transfer to the pyrolysis vessel were operations re- quiring great care in manipulation and the use of an inert atmosphere. These hazardous operations are eliminated ABSTRACT OF THE DISCLOSURE by the process of the present invention. In adition to im- This invention relates to a novel process for the prepa- 15 provements in safety, the process of the present invention ration of beryllium hydride. More specifically, it relates results in a marked increase in the speed of operation be- to a process wherein a beryllium alkyl is prepared by a cause of the large saving in time accompanying the elimi- novel method and, without separation from the reaction nation of the separation and transfer steps. system, is pyrolyzed to produce beryllium hydride. The invention will be more fully understood by refer- 20 ence to the following set of illustrative examples in which all parts and percentages are by weight. Beryllium hydride has been synthesized by Coates and Glockling [J. Chem. Soc. 1954, 2526] by the pyrolysis of EXAMPLE I ditertiary butylberyllium etherate and by Head, Holley A mixture of 10 parts of beryllium chloride bis (diethyl and Rabideau [J. Am. Chem. Soc. 79, 3687 (1957)] using 25 etherate) and 24 parts of triisobutyl aluminum was heated ether-free ditertiary butylberyllium. More recently, a su- at 50° C. for 30 minutes; a small amount (25 parts) of perior product has been obtained by the pyrolysis of di- diethyl ether was then added. This mixture was then intro- tertiary butylberyllium etherate dissolved in a high-boiling duced over a period of about 30 minutes into a high-boil- inert solvent (co-pending application Ser. No. 176,865, ing kerosene ("Bayol D") maintained at a temperature filed Feb. 26, 1962). 30 of about 190-195° C. After addition was complete, the An object of this invention is the provision of a novel mixture was cooled and filtered. The residue on the filter and improved method for the preparation of beryllium was washed several times with pentane and dried. Analysis hydride. Another object of this invention is the provision of the product by acid hydrolysis and measurement of of a method for the preparation of beryllium hydride the evolved hydrogen indicated beryllium hydride of a which is characterized by simplicity and rapidity of oper- 35 purity of about 72 percent. ation. Still another object of this invention is the provision When dodecane or tetralin was used in place of the of a method for the preparation of beryllium hydride high boiling kerosene, similar results were obtained. from berryllium halide which does not require the isola- tion of a beryllium alkyl intermediate. Other objects will EXAMPLE II appear hereinafter. 40 Sodium aluminum tetraisobutyl (16.7 parts) and 6.8 In accordance with the present invention it has been parts of beryllium chloride bis-diethyl etherate were com- found that beryllium hydride can be prepared convenient- bined in 25 parts of toluene. The sodium chloride pre- ly and rapidly by means of a two-stage process without cipitated rapidly from the mixed solution. The sodium separation, between the stages, of intermediate reaction chloride was separated by filtration and was washed on products. In the first stage an organoaluminum compound, 45 the filter with successive small portions of toluene and specifically an aluminum trialkyl or an alkali metal alu- ether. White oil (100 parts) was heated to 220° C. and minum tetraalkyl, wherein the alkali metal has an atomic the combined filtrate and washings obtained as indicated number of 3 through 55 and wherein the alkyl group con- above were added slowly to the hot oil. The heating was tains from 4 to 10 carbon atoms, inclusive, is caused to continued for an additional 10 minutes, after which the react with a beryllium halide to form the corresponding 50 mixture was cooled and filtered. The beryllium hydride beryllium dialkyl. In the second stage, the reaction prod- on the filter was washed with hexane and dried under vac- uct of the first stage is heated without further treatment uum. A sample of the product was analyzed by acid hy- to decompose thermally the beryllium dialkyl contained drolysis and was shown to contain approximately 55 per- therein to beryllium hydride. The foregoing procedure cent of beryllium hydride. represents an embodiment of the present invention. 55 When the sodium aluminum tetraisobutyl of Example Another embodiment of the present invention is the use II is replaced by sodium aluminum tetra-n-butyl, similar of a butyl aluminum compound in the reaction of the first results are obtained. stage of the process. A preferred embodiment of the pres- ent invention is the use of sodium aluminum tetrad- EXAMPLE IE butyl), sodium aluminum tetra(isobutyl), tri-n-butyl alu- 60 Twenty-five parts of triisobutyl aluminum and 4 parts minum or triisobutyl aluminum in the reaction of the of powdered anhydrous beryllium chloride were heated first stage, because when the named compounds are used together at 50° C. for one hour. After the addition of 50 the reaction of the first stage occurs at "a temperature well parts of benzene, the mixture was boiled for two hours below that of the thermal decomposition of the beryllium under reflux. About three quarters of the beryllium chlo- alkyl intermediate. 55 ride reacted. The benzene was removed under vacuum, Another preferred embodiment is the use in the first and the residue was introduced into Bayol D at 190-200° stage of a solvent boiling in the range of from about 50 to C. The resulting mixture was filtered, and the residue was about 125° C., for example, toluene, and in the second washed with hexane and dried. Hydrolytic analysis indi- stage a solvent boiling in the range of about 150 to about cated beryllium hydride of 70.5 percent purity. 220° C., for example, dodecane. These solvent ranges 70 When the triisobutyl aluminum of Example III is re- are preferred because their use assures that the formation placed by tri-n-butyl aluminum, similar results are ob- of beryllium alkyl is essentially complete before it begins tained. 3,830,906 EXAMPLE IV mesitylene, and mixtures of the foregoing, such as petro- leum naphtha, gasoline fractions and kerosene. The high- Sodium aluminum tetramethyl (22 parts) and 23 parts boiling solvents are saturated aliphatic or aromatic hydro- of beryllium chloride bis-diethyl etherate are combined carbons boiling above 170° C. These solvents include n- in 50 parts of ether. Sodium chloride precipitates rapidly decane, n-undecane, n-tridecane, n-tetradecane, n-penta- from the mixed solutions. The sodium chloride is sep- decane, cetane, propyleycloheptane 1,3 - dimethylcyclo- arated by filtration and is washed on the filter with suc- hexane, l-methyl-2-isoamyl cyclohexane, l,3-dimethyl-5- cessive small portions of ether. The combined filtrate and isobutylcyclohexane, hemimellitene, prehnitene, isodurene, washings are treated with approximately their own vol- n-butyl benzene, p-cymene, and 1,3,5-triethyl benzene, or ume of hexane. Dimethylberyllium separates out as color- mixtures of any of the foregoing. less needles, which are washed with a small quantity of 10 The reactions of this invention may be carried out under hexane and dried. any atmosphere inert to both the reactants and products When the sodium aluminum tetramethyl of Example IV but dry nitrogen is preferred. Other suitable protective is replaced by the corresponding potassium, rubidium or atmospheres include hydrogen, carbon monoxide, helium, cesium compound, similar results are obtained. 15 neon, argon, krypton, and xenon. As indicated above, the original reactants or raw ma- The product of this invention is a white to grayish terials employed in the process of this invention are an white powder which has strong reducing properties. The organoaluminum compound and a beryllium halide. The bulk of the product is insensitive to water and air, although organoaluminum compound employed may be selected a small amount of hydrolysis (of the order of 10 percent) from a rather broad range of compounds varying widely does occur upon contact with water. When heated in an in composition. For example they may include trialkyl 20 inert atmosphere, the product is stable up to a temperature aluminum compounds and alkali metal aluminum tetra- of about 160° C. alkyl compounds. In both series of compounds the num- The beryllium hydride product of this invention is of ber of carbon atoms in each alkyl group can vary from 4 to 10 or more. Compounds containing alkyl groups with great value as a fuel component of solid propellants. It more than 10 carbon atoms, while operable to some ex- 25 also represents a convenient source of small storeable tent, are more difficult to decompose than those with quantities of hydrogen and of pure beryllium metal.
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