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United States Patent (19) 11 4,029,530 Kenney (45 June 14, 1977

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United States Patent (19) 11 4,029,530 Kenney (45 June 14, 1977 United States Patent (19) 11 4,029,530 Kenney (45 June 14, 1977 3,002,012 9/1961 Backensto ..................... 260/.435. A METHOD OF FORMING LEAD STYPHNATE 54 3,301,882 l/1967 Taylor ........................... 260/435 A AMMUNITION PRIMING MIXTURE 3,320, 104 5/1967 Stadler ................................ 149/24 (75 Inventor: Joseph F. Kenney, Bridgeport, Conn. Primary Examiner-Edward A. Miller 73 Assignee: Remington Arms Company, Inc., Attorney, Agent, or Firm-John H. Lewis, Jr.; Nicholas Bridgeport, Conn. Skovran; William L. Ericson 22 Filed: Feb. 12, 1976 (2) Appl. No.: 657,487 57 ABSTRACT Ammunition rim fire priming mixtures are commonly Related U.S. Application Data prepared by mixing normal lead styphnate, a sensitizer, such as tetracene, an oxygen donor such as lead nitrate, 63 Continuation-in-part of Ser. No. 489,704, July 18, and a frictionator such as ground glass. This invention 1974, abandoned. relates to such a mixture and to center fire priming (52 U.S. C. ................................... 149/28; 149/27; mixtures which consist of lead styphnate, tetracene, 149/24 inorganic fuels and barium nitrate and to a method of (51 Int. Cl.' ......................................... C06B 41/06 forming them and is characterized by the use of lead 58) Field of Search ........................ 149/24, 27, 28; styphnate which is formed in situ by the reaction of a 260/435 A water wet mixture of styphnic acid and a lead com pound such as lead oxide (litharge), lead hydroxide, 56) References Cited basic lead carbonate, or lead carbonate. Important UNITED STATES PATENTS advantages of this invention are reduced cost, im 1,443,328 1/1923 Herz .................................... 149/24 proved safety since it is unnecessary to prepare, precip 1999,728 4/1935 Herz ............................... 149/24 itate, or separately handle pure or relatively pure lead 2,150,653 3/1939 Franz ... ... 260/.435 A styphnate and improved percussion sensitivity of the 2,239,547 4/1941 Brun .................................... 149/24 resulting mixtures. 2,295,104 9/1942 Garfield .............................., 149/24 2,589,703 3/1952 Kenney ................................ 149/24 2,702,745 2/1955 Kenney ................................ 149/24 5 Claims, No Drawings 4,029,530 1 2 the charging equipment and were found to harden to an METHOD OF FORMING LEAD STYPHNATE undesirable degree preventing charging when the wet AMMUNITION PRIMING MIXTURE mixtures were stored for such periods as overnight. This application is a continuation-in-part of my appli in the commercial manufacture of styphnic acid, cation Ser. No. 489,704, filed July 18, 1974, and now resorcinol is first sulphonated with 90% sulphuric acid. abandoned. After the sulphonation is complete, nitric acid is added, the material nitrated and the styphnic acid precipi BACKGROUND OF THE INVENTION tated. Some investigators (Franz, Wilkinson and Ehr Normal lead styphnate (normal lead trinitroresorci lich U.S. Pat. No. 2,150,653) feel that when styphnic nate) is a well-known primary explosive which has been O acid is so manufactured on a commerical scale, small widely used for the manufacture of percussion primers amounts of nitrous and nitric oxides are present during for small arms ammunition and the like where it first the sulphonation. This, they felt, produces a dark came into use as a replacement for fuiminate of mer brown material which may include some or all of the cury. Normal lead styphnate is a very powerful, percus nitro derivatives of resorufin, the nitro derivatives of sion sensitive explosive which is also quite sensitive to 15 indo-phenol and the nitro derivatives of resaZurin. static electricity. The danger of handling it in pure, or I have also discovered that styphnic acid produced by relatively pure form, is such that it is normally handled one of the commercial processes contains a minor only in small quantities, kept wet, and in rubber con amount of sulphuric acid. When styphnic acid is dis tainers or "boats.' Even with these precautions it has solved in amyl alcohol and the amyl alcohol solution been known to detonate as the result of the stimuli of extracted with water several times, the water extracts shock, friction, static electricity, or exposure to sparks may be bulked together, evaporated to one-half vol or flame. ume, chilled, and the precipitated crystals of styphnic The normal lead styphnate of this invention is pre acid removed by filtration. Successive repetitions of pared in situ in a wet mixture of styphnic acid (trini this technique of evaporating the water extract, cooling troresorcine) and a lead compound such as lead oxide 25 it to precipitate any remaining styphnic acid, filtering (litharge), lead hydroxide, basic lead carbonate, or out the crystals, etc. followed by evaporation as far as lead carbonate. In the resulting wet mixture the lead possible in a steam bath and by evaporation in a vac styphnate does not show any undesirable sensitivity to uum oven at 65' C resulted in the concentration of a initiation by shock, friction, or static electricity and black oily residue. This oily residue was found to have such wet mixtures can be handled in normal primer 30 as its principal ingredient sulphuric acid which was charging operations with little or no risk of accidental undoubtedly carried over from the sulphonation pro explosion. cess. Other impurities are also present in the oily resi As set forth in Davis “The Chemistry of Powder and due and are believed to consist of one or more of the Explosives," Page 440, Vol. II (1943) John Wiley and impurities referred to in the aforementioned Patent No. Sons Inc.,lead styphnate is commonly prepared by add 35 2,150,653 or in a later patent to one of the same inven ing a solution of magnesium styphnate at 70° C. to a tors, Patent No. 2,246,963. well stirred solution of lead acetate at 70° C. A volumi As will be noted from these patents, it was theorized nous precipitate of the basic salt separates. The mixture that the presence of these impurities was helpful in the is stirred for 10 or 15 minutes; then dilute nitric acid is manufacture of lead styphnate and if the styphnic acid added with stirring to convert the basic salt to the nor 40 was too pure it was the practice of these inventors to mal salt and the stirring is continued while the tempera add one or more of such impurities or to modify the ture drops to about 30°C. The product, which consists process to insure that they would be produced. of reddish-brown, short, rhombic crystals, is filtered Certainly the presence of these impurities had no off, washed with water, sieved through silk, and dried. adverse effects in the formation of lead styphnate by In the processes of filtration and washing undesirable 45 the methods of the prior art for in the precipitation, impurities tend to be eliminated. filtering, washing and drying of the lead styphnate, the Other methods of producing normal lead styphnate impurities or lead salts formed from reactions with such are described in the patents of Edmund Herz, such as impurities, were readily separated from the dense crys No. 1443,328 and No. 1999,728, the latter process talline normal lead styphnate. having been used commercially for many years in the SO However, in the practice of applicant's process, making of many millions of small arms primers. This wherein the normal lead styphanate is precipitated in latter method is characterized by the preparation of situ in a priming mixture, there is no opportunity to lead styphnate by the interaction of a concentrated eliminate the impurities or any products resulting from solution of magnesium styphnate with a solution of lead a reaction with the impurities. Although the impurities nitrate in the presence of free styphnic acid. 55 do not interfere with the production of the lead styph The patent to Brun No. 2,239,547 proposes to make nate, by remaining in the mixture they profoundly af. a priming mixture by mixing moist mono-basic lead fect the resulting mixture and it may become so sticky styphnate with moist styphnic acid and other priming that it adheres to tools and charging plates and hence mixture ingredients such as a sensitizer, an oxidizer, cannot be charged into primers in the usual way and and an abrasive. However, mono-basic lead styphnate 60 the mixtures may harden up so quickly that they cannot is itself a dangerously sensitive primary explosive and be stored for the required length of time or handled in by practicing the Brun invention it would not be possi the normal manner. ble to achieve the chief advantages of applicant's Accordingly, when referring to lead styphnate for use method as later hereinafter set forth. in my invention, I refer to relatively pure styphnic acid When the first attempts were made to produce lead 65 in the form of dense crystals of reasonably uniform styphnate in accordance with the present invention, shape and size and of the light color associated with the commercial styphnic acid was used and the resulting pure product. The dark brownish commercial styphnic mixtures were found to be so sticky that they clung to acid or any other form of styphnic acid containing 4,029,530 3 4 significant amounts of impurities such as sulphuric in the reacting mass unless it can be established that acid, the nitro derivatives of resorufin, the nitro deriva such ingredients do not themselves react with one or tives of indophenol and the nitro derivatives of res the other of the reactants or with any intermediate aZurin should not be used. compounds which may be formed. Thus, it has been As has been indicated, there are known prior art 5 established that gum arabic in water solution which is methods of producing styphnic acid of the desired pu usually employed as a binder in wet priming mixtures, rity and the usual commercial styphnic acid may be may be present while the reaction is going on, does not adequately purified by dissolution and re-crystalliza enter into that reaction, and may be desirable through tion.
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