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UNITED STATES PATENT OFFICE 2,559,684 STABILIZING RED PHOSPHORUS Sol Skolnik, Inyokern, Calif., and Grover L

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UNITED STATES PATENT OFFICE 2,559,684 STABILIZING RED PHOSPHORUS Sol Skolnik, Inyokern, Calif., and Grover L Patented July 10, 1951 2,559,684 UNITED STATES PATENT OFFICE 2,559,684 STABILIZING RED PHOSPHORUS Sol Skolnik, Inyokern, Calif., and Grover L. Bridger, Ames, Iowa, assignors to Tennessee Walley Authority, a corporation of the United States No Drawing. Application April 27, 1949, Serial No. 90,035 3 Claims. (C. 23-223) (Granted under the act of March 3, 1883, as amended April 30, 1928; 370 C. G. 75) 2 The invention herein described may be manu are ineffective for stabilizing red phosphorus factured and used by or for the Government for against accidental ignition due to impact and governmental purposes without the payment to friction. us of any royalty therefor. It is highly desirable that some method be pro This invention reiates to improved methods vided which will stabilize red phosphorus against for stabilizing red phosphorus against ignition accidental ignition under the influence of im caused by impact or friction, particularly effec pact and friction, and which will leave red phos tive in stabilizing freshly prepared red phos phorus powder in an apparently dry and free phorus against the hazards of impact or friction flowing. State. It is also desirable that any such ordinarily encountered in handling or shipping 10 method should leave no foreign substance in the the dry material. red phosphorus which is not easily removable by Although red phosphorus is a relatively stable simple Washing With water. It is also desirable material as compared with yellow phosphorus, that a method be provided which not only re the handling and shipping of red phosphorus are duces the danger of ignition of red phosphorus attended by a number of hazards. Red phoS 15 under impact or the influence of friction, but phorus does not ignite Spontaneously on expoSUlre which also retards oxidation of traces of yellow to air unless it contains appreciable traces of phosphorus which are frequently present. yellow phosphorus. Such traces of yellow phos. It is an object of this invention to provide a phorus are frequently present in freshly manu method for stabilizing finely divided red phos factured red phosphorus. Even Substantially 20 phorus against ignition under impact or the in pure red phosphorus can be easily ignited when fluence of friction and which will leave such red it is handled in Such manner that there is Sub phosphorus powder in an apparently dry and stantial impact on the mass of particles or con free-flowing state. - siderable friction is imposed upon them. Such Another object is to provide such method which conditions are frequently encountered in the 25 will not result in the incorporation of any mate packaging and shipping of red phosphorus SO rial in stabilized red phosphorus which is not that the danger of fire is always present. easily removable by simple washing with water. it has long been known that red phosphorus Another object is to provide an apparently dry, slowly oxidizes in the air, and in the presence of free-flowing red phosphorus powder stabilized moisture normally present in air, phosphoric acid 30 against ignition under impact or the influence of is formed. This is shown by A. W. Melor's friction. treatise on Inorganic and Theoretical Chemistry, Other objects and advantages will become ap vol. 8,772 (1928). Upon such exposure to air with parent as this disclosure proceeds. partial oxidation and formation of phosphoric We have now found that finely divided red acid, a mass of finely divided red phosphorus be phosphorus normally susceptible to ignition under comes moistened with hygroscopic acid and cakes the influence of impact and friction may be sta into a mass which is difficult to handle. bilized by depositing a small quantity of a mate So far as is known, there are no methods dis rial selected from the group consisting of phos closed in the prior art for reducing the danger phorus pentoxide, phosphorus trioxide, highly of ignition of red phosphorus under impact or concentrated phosphoric acid, highly concen friction. In fact, for most uses, it is desired that 40 trated phosphorous acid and mixtures thereof, as this material be sensitive to impact or friction. a coating upon the surfaces of the individual par Prior efforts, therefore, have been directed to the ticles of such red phosphorus and maintaining stabilization of red phosphorus against Slowy Sur the resulting coated red phosphorus in a condi face oxidation without materially reducing the tion of apparent dryness. sensitivity of the material toward ignition under The above-mentioned oxides and acids of phos the influence of impact or friction. To this end phorus may be deposited as a coating upon indi it has been proposed to treat red phosphorus vidual particles of red phosphorus in a number with a small amount of a lyophilic protein-con of different manners. When using a material taining colloid and to dry under conditions such 50 selected from the group consisting of concern that a thin film is deposited around the indi trated phosphoric and phosphorous acids, we pre vidual particles. Coating red phosphorus parti fer to incorporate the acid into the mass of red cles with aluminum hydrate by aeration of a phosphorus powder in any manner which results slurry of red phosphorus in a soluble aluminate in substantially even distribution of acid and solution also has been proposed. Such coatings 55 dry the resulting coated phosphorus to a state 2,559,684 3 4. of apparent dryness at a low temperature-pref sample of finely divided red phosphorus was erably about 60° C. Ordinary concentrated treated with concentrated phosphorous acid in phosphoric or phosphorous acid of commerce are proportion equivalent of 13 per cent, calculated as used, and these acids become highly concentrated P2O5, of the weight of the phosphorus. This ma by such drying. terial also was dried to apparent dryness at low When an oxide of phosphorus is used, prefer temperature. ably phosphorus pentoxide, we prefer to pass the 4. Another portion of the above sample Was oxide in very finely divided form Suspended in a coated with phosphorus pentoxide in an ex gas through a bed of red phosphorus powder for tremely finely divided state, passed through a bed a time sufficient to deposit the required coating on 0 of the finely divided phosphorus until the per the surfaces of the individual particles of red cent of P2O5 deposited thereon amounted to 6.7. phosphorus. 5. The portion of sample described in para The amount of oxide or acid necessary to mate graph 4 above, after treatment with phosphorus rially increase the stability of red phosphorus pentoxide, was divided and one part was treated against ignition by impact and friction is Small. 5 with lime in proportion sufficient to neutralize As little as 1 to 3 per cent of Such oxide or acid, the phosphorus pentoxide. calculated as P2O5, has been found to materially 6. A small sample of red phosphorus WaS pre increase the resistance of red phosphorus to ig pared, containing no iron, copper, oxide, or acid. Inition by impact and friction. We prefer how Pellets were prepared from each of the above ever to use a quantity between 5 and 7 per cent, 20 treated samples and these pellets Were tested in calculated as P2O5, as this amount is sufficient to the impact machine described above. The ball impart to the red phosphorus a high degree of was dropped from the maximum height of the stability without any change in its property of machine-29 inches-successively onto 25 pellets being free-flowing and noncaking. The addition prepared from each given portion, and the num of quantities of oxide or acid above 7 per cent 25 ber of pellets that fired and failed to fire Was adds very little to the stability of the phosphorus, noted. The procedure was repeated from lower and the addition of very large quantities detracts heights at 2-inch intervals until none of the somewhat from the free-flowing quality of the pellets fired. A graph was plotted with "fraction phosphorus. Considerably more than 7 per cent, misfired' as abscissae and “height' as Ordinates. however, may be added without causing the ma 30 The height at which the curve crossed the One terial to cake; provided that very high concen half misfired line was taken to be the average tration of acid is maintained. Substantially all height. Results of these tests are given in the uncombined water should be removed in the dry. following table. ing step mentioned above. Table I After coating the particles of phosphorus pow 35 der, it is necessary that they be maintained in a State of apparent dryness. The oxides or acids Grams as Average used are highly hygroscopic and tend to absorb numberPortion Treatment gramP2O5 perred height, moisture from the air, thereby causing the phos phosphorus phorus to become sticky and to cake. One pre 40 1--------- Free of oxides and acids--------- () 11.3 ferred method of maintaining such phosphorus in 2--------- Coated with concentrated phos- 0.050 26.2. a state of apparent dryness is merely to pour phoric acid and dried. 3. -------- Coated with concentrated phos- 0.30 28.7 the free-flowing powder into drums until the phorous acid and dried. drums are substantially filled and then to close 4--------- C with phosphorus pent- 0.067 25. Of OX3. the openings thereof. Such phosphorus may be 5--------- Coated with phosphorus pent- 0.067 4.3. shipped in closed containers with little of the 45 oxide -- line. usual hazards encountered in shipping such ma 6.-------- Free of oxides, acids, Fe and Cul-- G .5 teria. When it is desired to remove the phos phorus from such containers, it may be poured From the above table it is apparent that the out easily, conveniently, and quickly.
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