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United States Patent 0 1 3,269,879 United States Patent 0 ICE Patented August 30, I966 1 2 ammonium nitrate, and substituted in said lattice inor 3,269,879 AMMONIUM SALT LATTICE WITH ISOMOR ganic salts isomorphously co-crystallizable therewith. PHOUSLY SUBSTITUTED INORGANIC SALTS These inorganic salts are sometimes hereinafter referred Manfred Stammler, Carmichael, and Wilfred G. Schmidt, to as substituent salts. Sacramento, Calif., assignors to Aerojet-General Corpo 5 The inorganic salts capable of undergoing cocrystalliza ration, Azusa, Calif., a corporation of Ohio tion with ammonium perchlorate to form isomorphous No Drawing. Filed Apr. 13, 1964, Ser. No. 359,511 compositions include those having the formula: 16 Claims. (Cl. 149—2) (1) Maxi: This invention relates to novel isomorphous ammonium w'herein M is an alkali or alkaline earth metal cation, perchlorate and ammonium nitrate compositions prepared or the ammonium (NH4) group, and has a valence nu by cocrystallization, having greater sensitivity to impact merically equal to “12"; and X is an anion selected from and lower decomposition temperature, and being especial the group consisting of chromate, iodate, periodate and ly useful in explosive compositions, and to the method of permanganate, and has a valence numerically equal to producing the same. 15 “a.” Subscripts “a” and “b” are small whole numbers An explosive in the broadest sense, is a material which, of from 1 to about 3. Compounds within the scope of under the in?uence of shock, decomposes rapidly and Formula I include sodium chromate, lithium iodate, potas spontaneously with evolution of large amounts of heat sium periodate, calcium permanganate, strontium chro and gas. The hot gases create extremely high pressure mate, magnesium iodate, barium chromate, ammonium if the explosive is set off in a con?ned space. Today, 20 chromate, ammonium periodate and ammonium perman explosives are used to perform many engineering feats ‘ganate. which would be physically or economically impossible Another class of compounds which can be effectively without their use. Many diiferent types of explosives cocrystallized with ammonium perchlorate are those hav ‘have been employed for these purposes. Explosives vary ing the formula: widely in their sensitivity and power. Ordinarily explo 25 sives are classi?ed in one of the following three catagories; (II) M'cX'd initiating explosives such as mercury fulminate and lead wherein M' is a thallium, silver or copper cation; the azide; high explosives such as cyclo-trimethylenetrinitra valence of M’ is equal numerically to “d”; X’ is an anion mine (RDX); and low explosives such as black powders. selected from the group consisting of perchlorate, chro The initiating explosives are quite sensitive materials mate, iodate, periodate and permanganate; and has a which can be made to explode by the application of ?re valence equal to “c.” Subscripts “c” and “d” are small or by means of a slight blow. Initiating explosives are integers, usually equal to 1, 2 or 3. Compounds of the generally used in primers and detonators. High explo type de?ned by Formula II include thallium perchlorate, sive materials are those capable of exploding with great silver iodate, copper periodate, silver chromate, thallium , violence when set oil by an explosive shock such as that 35 iodate, copper permanganate and silver perchlorate. which would be obtained by detonating a small amount The ammonium nitrate is cocrystallized with com of initiating explosive in contact with the high explosive. pounds of the formula: The low explosives diifer in their mode of decomposition from the other two types, in that they only burn, and thus (III) M"eX"; their action is less shattering. 40 wherein M" is a cation selected from the group consist The bulk of the explosives employed industrially in ing of silver, thallium, copper, or an alkali metal such the United States in mining and construction work is of as potassium, lithium or sodium. The valence of M" the high explosive type. However, many of the high ex numerically equals the value of “f.” In this formula, plosives commonly used, such as RDX, are relatively ex X" is an anion having a valence equal to “e” and is se pensive. ’Dherefore, lower cost ingredients for high ex lected from the group consisting of nitrate, permanganate plosive compositions are needed. Ammonium perchlo 45 and Z”O3 where Z" is halogen, preferably chlorine, rate and ammonium nitrate are well-known as oxidizer bromine or iodine; and “e” and “f” are integers of from materials for use in solid rocket propellants. However, 1 to about 3. The inorganic salts capable of being co these materials are relatively insensitive to impact, thus crystallized with ammonium nitrate and de?ned by For limiting their use in high explosive compositions. It has mula III, include silver nitrate, thallous nitrate, potassium now been found, however, that the sensitivity to impact 50 permanganate, potassium chlorate, potassium br'omate and of ammonium perchlorate and ammonium nitrate can be potassium iodate. increased to a level approximately corresponding to that In Table I there appears illustrative isomorphous com possessed by RDX. This has now been accomplished by positions within the scope of our invention. cocrystallizing ammonium perchlorate and ammonium TAB LE I nitrate with certain other inorganic salts. These cocrystal 55 lized salts are isomorphous in nature and possess greater Lattice substituent Salt sensitivity to impact. It is therefore an object of this invention to provide ammonium perchlorate and ammonium nitrate composi Amiéionium Perehlorate_ . Sodium Chromate. 0 Potassium Chromate. tions possessing substantially enhanced impact sensitivity. Calcium Iodate. Still another object of this invention is to increase the low Potassium Periodate. _ Copper Permauganate. temperature decomposition rate of ammonium nitrate Thallium Perchlorate. and ammonium perchlorate. More speci?cally, it is an Silver Chromate. Potassium Iodate. object of this invention to provide novel impact sensitive Magnesium Periodate. compositions containing a lattice of ammonium perchlo Potassium Permanganate. Silver Nitrate. rate or ammonium nitrate and containing isomorphously Thallous Nitrate. substituted therein certain inorganic salts. These and Potassium Permanganate. Potassium Chlorate. other objects of this invention will become apparent from Potassium Bromate. the detailed description which follows. Potassium Iodate. There has been found according to this invention novel impact sensitive compositions comprising a lattice selected The substituent inorganic salts are normally .present in from the group consisting of ammonium perchlorate and the isomorphous cocrystallized compositions in the 1 3,269,879 3 A. amount of from about 0.1 percent to about 10 percent Was obtained, the precipitate was ?ltered, dried, and by weight and more preferably ‘from about 0.5 percent screened, to obtain an isomorphous cocrystallized prod .to about 2 percent by weight, ‘based on the total weight uct. The product obtained by the above-described meth— of the cocrystallized product. The ?nal isomorphous od was analyzed for concentration of the inorganic salt cocrystallized product is in a single phase and has an chemically. The results are as follows: average particle size of from about 20 microns to about 700 microns. NH4C-lO4-CaOrO4—2.03 percent by weight CaCrO4 Normally, the cocrystallization is carried out by ?rst tfound. dissolving the ammonium perchlorate or ammonium ni EXAMPLE HI trate and the inorganic salt to be cocrystallized therewith 10 Cocrystallized ammonium perchlorate and in water, and thoroughly mixing the solution. At least potassium iodate some of the water is then removed by heating and/or A 490 gram sample of ammonium perchlorate was dis the application of reduced pressure until cocrystalliza solved in about 3 liters of water. The solution was poured tion occurs. Preferably, this ‘concentration procedure into a 3-neck ?ask provided with a stirrer, thermometer is carried out at a temperature of ‘from about 20° C. to 15 and a dropping funnel. A solution of 10 grams of potas about 100° C., and at a pressure of from about 0.01 to sium iodate in 500 ml. of water Was then slowly added about 1 atmospheres. to the aqueous ammonium perchlorate solution. "The The weight ratio of total salts to water in the aqueous vigorously stirred mixture was then concentrated at 50° solution prior to concentration may be varied over a C. under reduced pressure. When a thick slurry was wide range and is not critical. Generally there should 20 obtained, the precipitate was ?ltered, dried and screened, be initially present su?icient water to dissolve all of the to obtain an isomorphous cocrystallized product. The salts. It can be seen that the minimum amount of water product obtained by the above-described method was required for a given weight of salts will depend on the analyzed and ‘found to contain about two percent potas solubility of the salts and the mixing temperature being sium iodate. employed, and thus is readily ascertained by those skilled 25 EXAMPLE IV in the art. Ordinarily, the amount of water used will be somewhat in excess of the minimum amount, and will Cocrystallized ammonium perchlorate and be from 0.2 to about 20 times the weight of the total potassium periodate salts. While the foregoing discussion is limited to the A 490 gram sample of ammonium perchlorate was dis— use of water as to the solvent, it is to be understood that solved in about 3 liters of water. The solution was poured any substantially inert solvent in which the salts are at into a 3-neck ?ask provided with a stirrer, thermometer least somewhat soluble may be utilized. Illustrative of and a dropping funnel. A solution of 10 grams of potas other suitable solvents are the lower alkanols such as sium perchlorate in 500 of water was then slowly methanol and ethanol, and .the lower alkylene glycols added to the aqueous ammonium periodate solution. The such as ethylene glycol and propylene glycol.
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