, 2,962,358 zllniit?dstates Patent‘ ” ICC. Patented Nov. 29,1969

7 l . , r 2 . percent recovery of the theoretical amount of lithium peroxide available-can be obtained. 2,96%“ The drying may bedone underatmosphen'c pressure at 1 METHOD on MAKING LITHIUM PERoxmE suitable temperatures to keep decomposition of the lithium IN METHANOL peroxide at a ' ‘Ethyl alcohol can be used, as well as methanol, and Henry H. Strater, May?eld Heights, Ohio, assignor to commercial strength alcohols are satisfactory. The re 8: Chemicals, Willoughby, Ohio, a corporation action of the invention will occur at room tempera 0 o ture. No Drawing. Filed June 2, 1958, Ser. No. 738,959 10 Should it be desired to recover the lithium present in the end ?ltrate material, the ?ltrate can be heated to 4 Claims. (Cl. 23-184) distill the alcohol therein which can be recovered for further use. The water present also is evaporated o? and the residue material will have been partially con The present invention relates to a method of preparing 15 verted from lithium peroxide over to lithium hydroxide. lithium' peroxide, and particularly relates to the prepara Such end product can be puri?ed in any conventional tion of such material in an alcohol reacting medium. manner and be again used in the practice of the process, Heretofore there have been some methods proposed or it can be used for other purposes, as desired. for the production of lithium peroxide, vbut none of such The reaction conditions are readily controllable by methods have been completely satisfactory for low cost 20 the process described, as the hydrogen peroxide is slowly eifective production of lithium peroxide, so far as I am added to the reacting materials and no excessive tem aware. More uses are being found for lithium peroxide peratures would be produced. The reacting materials as an oxygen source because it is a low weight solid can be cooled in any conventional manner, if desired. and need exists for a relatively uncomplicated method The process of the invention can be readily practiced by which the desirable quantities of lithium peroxide 25 and the end product, lithium peroxide, is ready for use can be economically and safely secured. for any desired purpose. It thus can be used as a solid The general object of the present invention is to pro fuel, asfor a rocket, or it is possible to use the lithium vide a novel and improved method of producing lithium peroxide as a source of oxygen for other purposes. peroxide by the oxidation of a solution of anhydrous From the foregoing description, it will be seen that lithium hydroxide in an alcohol by use of hydrogen 30 the invention has provided an easily practiced safe proc peroxide as an oxidizing agent. ess for producing lithium peroxide so that the objects Another object of the invention is to provide a safe, of the invention have been achieved. easily practiced process for obtaining an end product While one complete embodiment of the invention has having a high percentage of lithium peroxide content. been disclosed herein, it will be appreciated that modi Another object of the invention is to utilize the in 35 ?cation of this particular embodiment of the invention solubility of lithium peroxide in alcohol to facilitate may be resorted to without departing from the scope the formation of commercial percentages of lithium per of the invention as de?ned in the appended claims. oxide in a reversible chemical reaction. What is claimed is: The foregoing and other objects and advantages of 1. A method of preparing lithium peroxide consisting the invention will be made more apparent as the speci 40 of the steps of dissolving su?‘icient anhydrous lithium ?cation proceeds. hydroxide in methyl alcohol to saturate the solution, said The present invention, in general, relates to the pro anhydrous lithium hydroxide containing lithium carbo duction of lithium peroxide by dissolving anhydrous lith nate as an impurity and which impurity is insoluble in ium hydroxide in an alcohol solution until the solution is methyl alcohol, ?ltering off any insoluble materials in saturated, ?ltering off any insoluble materials, such as 45 cluding the lithium carbonate, adding hydrogen perox carbonates present in the solution, adding hydrogen perox ide solution slowly to the lithium hydroxide solution and ide solution slowly to the lithium hydroxide solution and stirring the mixed solutions, permitting the mixed solu~ stirring the mixture, during which time the lithium per tions to react at the ambient temperature, lithium perox oxide is produced as a precipitate, and thereafter ?ltering ide being produced as a precipitate, ?ltering the mixed the mixed solutions to recover the lithium peroxide end 50 solutions to remove the lithium peroxide therefrom, product. washing the lithium peroxide with methyl alcohol and Example drying the washed lithium peroxide under vacuum. One example of the process of the invention comprised 2. A method as in claim 1 wherein the ?ltrate after the dissolving of 500 grams of anhydrous lithium hydrox removal of the precipitated lithium peroxide still con ide in 7500 cc. of commercial 95% methanol. The solu 55 tains lithium peroxide in solution, the additional steps tion was then ?ltered to remove insoluble lithium car of heating the solution to distill the alcohol therefrom bonate and other insoluble materials present. Approxi and to form lithium hydroxide from the lithium perox mately 3000 cc. of 27.5% hydrogen peroxide was slowly ide, and recovering such lithium hydroxide for further added over a period of about 10 minutes to the lithium processing. hydroxide solution while the mixture was stirred. Then 60 3. A method of preparing lithium peroxide consist the mixture was permitted to react for approximately ing of the steps of dissolving su?icient anhydrous lithium thirty minutes and occasionally stirred during such re hydroxide in an alcohol from the class consisting of action time. A precipitate of lithium peroxide was pro methanol and ethanol to saturate the solution, ?ltering duced and the reaction mixture was ?ltered to obtain off any insoluble materials, adding hydrogen peroxide the lithium peroxide. Such end product was washed slowly over an interval of several minutes to the lithium twice with 100 cc. portions of commercial 95% men hydroxide solution while stirring, lithium peroxide being thanol. The product was dried in a vacuum of 29" produced as a precipitate in the reaction mixture, ?lter at between 90 to 100° C. and 380 grams of 96.0% lithium ing the solution to remove the lithium peroxide there peroxide were recovered. from, washing the lithium peroxide with the solution In the practice of this process, the strength of the 70 alcohol, and drying the washed lithium peroxide. hydrogen peroxide used can be changed and with the 4. A method of preparing lithium peroxide from ma higher percentage solutions of such peroxide, a greater terials in the proportions indicated and consisting of the 2,962,358

, r V - 3 - e 4 steps of dissolving about 500 grams of anhydrous lithium lithium peroxide therefrom, and drying the lithium perox hydroxide in about 7500 cc. of methyl alcohol to sat- ide. urate the solution, ?ltering off any insoluble materials, adding. about 3000 cc.‘ of a 27.5% hydrogen peroxide References Cited in the ?le of this patent ‘solution slowly to the lithium hydroxide solution while 5 stirring, letting the mixed solutions stand and react for UNITED STATES PATENTS about 30 minutes, lithium peroxide being produced as 2,215,856 P?eiderer ______Sept. 24, ‘1940 a precipitate, ?ltering the reaction solution to remove the 2,438,485 Winternitz ______Nov. 15, 1949