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United States Patent Office Patented Sept. 5, 1944 2,351,655 UNITED STATES PATENT OFFICE 2,357,655 - PROCESS FOR THE MANUFACTURE OF STRONTIUM PEROXIDE August Hummel'. Bernardsville, and William M. Driesen, Clifton, N. 1., assignors to Hnmmcl Chemical Company, Inc., New York, N. Y., a corporation of New York No Drawing. Application September 154, 1942, Serial-No.458,468 , 11 Claims. (Cl. 23-187) ‘ , Strontium peroxide is known to exist ‘in sev in any suitable apparatus in the shortest possible eral forms. One form is made by‘the so-called time to avoid excessive loss of available oxygen. wet process of production and is identi?ed by ' The mass resulting from the sintering opera its very low density and its light, ?uffy, powdery tion is. in‘ the form of irregular hard lumps of physical characteristics. Another form made by varying sizes, each containing a mixture of about direct oxidation of ‘strontium oxide is completely 30% to 50% anhydrous strontium peroxide and , different in its physical characteristics and com 70% to 50% of strontium oxide, the ratio being prises discrete particles of granular or sandy dependent upon the time and temperature of character and of much greater density and is sintering. 7 free-?owing. The-ratio of the densities by vol Example I ume of the ?uffy and granular forms of the ma Hydrated strontium peroxide resulting from . terial is as 1:5 approximately. the reaction de?ned above and in dried powdery United States Patent 1,325,043 to James B.‘ form was sintered for ten minutes at a tempera‘ Pierce refers to the ?rst form of the material as ture of 350° F. and the product analyzed to indi having certain objections and discloses a method cate 50% strontium peroxide and 50% stron-_ of making the second form comprising the direct tium oxide. oxidation of strontium oxide. This process in volves pressures up to eighteen :hundred pounds ‘ ' Example I! per square inch and temperatures up to 500° C. Hydrated strontium peroxide resulting from and is hence costly, dangerous, and wasteful. the reaction de?ned above and in dried powdery The present invention contemplates an im form was sintered for ten minutes at a tempera proved method for the manufacture of stron ture of 500° F. and the product analyzed to tium peroxide in-which pressures above atmos indicate 30% strontium peroxide and ‘70% stron pheric are not required and in which there is tium- oxide. 7 no loss of free oxygen. The process is charac 25 It will be noted here that the sintering opera terized by its extreme simplicity and low cost of tion' produces two important results, ?rst, it en operation and minimum requirements for appa tirely eliminates the water of crystallization, and ratus and materials. _ secondly, it combines the small powdery particles In accordance with the ‘present invention it is into larger denser ones. ' preferred to manufacture the strontium peroxide 30 Strontium peroxide is insoluble in water and from strontium nitrate of‘ good commercial qual at low temperatures does not react with the same ity by mixing it with sodium peroxide in molec while strontium oxide readily combines with ular proportions. For e?ceting this reaction it water to form strontium hydroxide in its hy is advantageous to use a saturated aqueous solu drated form (Sr(OH) 2.81120). This material is tion of strontium nitrate into which the sodium dif?cultly soluble in water at 32° F. but its peroxide in granular form is introduced grad solubility increases about ?fty times at 212° F. ually. The temperature of this reaction is main In order to separate the sintered mixture of tained below 135° F. by any suitable means to strontium peroxide and strontium oxide, the avoid decomposition of the strontium peroxide whole mass in its heated condition is rapidly formed. 40 quenched in a quantity of water greatly inex The chemical equation of the reaction is as cess of the amount necessary to convert the oxide follows: ' ' ' ' into the hydrated hydroxide. Since it is essen tial to control the temperature, of the exothermic I reaction resulting from. the formation and solu The strontium peroxide produced in this re 45 tion of the hydroxide, this quantity of water may action is in a complex hydrated form. The well be regulated‘ for that purpose. The tern; . strontium peroxide is insoluble in water and is . perature of the water can be that most easily‘ precipitated while the sodium nitrate formed is available, say from 50° F. to 75° F. The reaction in solution in the excess water and can be re preferably is maintained at a temperature not moved by decantation or by any other means. 50 substantially higher than 120° F. If it is not de The-hydrated strontium peroxide is now dried sired to use a substantially greater quantity of by mechanical means to eliminate its uncom water than that necessary to form and dissolve bined water and the dry powder is sintered by ' the ‘hydroxide, then some effective form of tem heating at a temperature preferably between perature control of the water into which the sin 2 2,357,055 The strontium peroxide will settle out at the 5. The method of producing strontium ,per bottom and the solution or strontium hydroxide < oxide from hydrated strontium peroxide com may be decanted 011 or otherwise separated. The prising sintering the hydrated strontium per strontium peroxide is then washed with water oxide at a temperature not substantially greater to remove all of the adherent strontium hydrox than 500° F. and for a period not substantially ide. The surface moisture adherent to the stron longer than ten minutes to convert the same to tium peroxide is now removed in a vacuum dryer a mixture of strontium oxide and a substantial . to avoid loss of available‘oxygen and the mate percentage of , anhydrous strontium peroxide, rial is then ready for use. _ quenching the sintered mass to convert the oxide The strontium hydroxide solution is treated 10 to the hydrate, dissolving the hydrate in water, separately with the molecular amount of hydro separating the peroxide from the solution, and gen peroxide which reacts with the same to form‘ drying the same at low temperature for use. hydrated strontium peroxide. This material is >6.‘The method of producing strontium per precipitated and separated from the liquid and oxide from hydrated strontium peroxide com returned to the process for subsequent conversion 15 prising sintering the hydrated strontium peroxide tothe anhydrous peroxide. at a temperature not substantially greater than It will be obvious that the reaction ?rst men 500° F. and for a period not substantially longer tioned herein uses‘ sodium peroxide as a con than ten minutes to convert the same to a mix venient source of oxygen to combine with the ture of. strontium oxide and a substantial per strontium from the nitrate. Other suitable mate 20 centage of anhydrous strontium peroxide. rials may be used. Likewise strontium nitrate is quenching the sintered mass in such excess quan not necessary as a starting material. The essen-, tity of water as to convert the oxide to the hy tial part of the process resides in thetreatment ‘ drated hydroxide, dissolve the latter and to hold of. the hydrated strontium peroxide, however ob . the heat of reaction and solution to a tempera— tained, to convert it to the anhydrous’ form. 25 ture not substantially greater than 135° F., sepa The strontium peroxide produced by the meth rating the peroxide from the solution, and drying od de?ned above shows a very high density and _ the same. can be mechanically reduced to a free-?owing 7. The method of producing strontium per~ granular material ‘of sandy, discrete particles. oxide from hydrated strontium peroxide com The material in this form is highly desirable for 30 prising sintering the hydrated strontium peroxide the production of red ?ames in pyrotechnic and ' at a temperature between 350° F. and 500° F. for military compositions. Tracer bullets require the a period of approximately ten minutes to convert material in this form as an ingredient of the the same to a mixture of from 30% to 70% of tracer composition.- I anhydrous strontium peroxide and 70% to 30% Having thus described the invention, what is 35 of strontium oxide, converting the oxide to lay-4 claimed as new and desired to be secured by Let droxide by reacting the mixture with water, dis ters Patent is: solving the hydroxide, separating the peroxide 1. The method of manufacturing strontium from the solution, washing the peroxide, and dry peroxide which. consists in reacting strontium ing the same in vacuum at room temperature. nitrate and sodium peroxide to form hydrated 40 8. The method of producing strontium per sintering the dried peroxide to convert the same oxide'which consists in reacting a strontium salt strontium peroxide, removing uncombined water and. a peroxide capable of forming hydrated to anhydrous strontium peroxide and strontium‘ strontium peroxide, drying the peroxide,’ sinter oxide, quenching the sintered material in water ing the same to form a mixture of anhydrous per to convert the oxide to hydroxide and to dissolve 45 oxide and oxide of strontium, separating the the latter, removing and drying the anhydrous mixture by the use of water, washing, and dry strontium peroxide. ing the strontium peroxide. ~ 2. The method of manufacturing strontium 9. In the method of claim 8 in which the water peroxide which consists in reacting strontium ni treatment results in a solution of strontium hy trate and sodium peroxide to form hydrated -50 droxide, treating this solution with hydrogen per strontium peroxide, removing uncombined oxide to form a precipitate of hydrated strontium water, sintering the dried peroxide to con peroxide, separating and drying the, precipitate, vert the same to anhydrous strontium peroxide and returning it to the sintering stage.
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