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United States Patent (19) 11 Patent Number: 5,682,004 Fels Et Al

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United States Patent (19) 11 Patent Number: 5,682,004 Fels Et Al III US005682004A United States Patent (19) 11 Patent Number: 5,682,004 Fels et al. 45 Date of Patent: Oct. 28, 1997 54) APPARATUS FOR REDUCTION OF THE 4,124,663 11/1978 Brantley et al. ......................... 264/3.5 GRAN SZE OF CRYSTALLINE EXPLOSVE 4,150,900 4/1979 Smith, Jr. et al. ... 366/302 4,657,607 4/1987 Perotto et al. ....... ... 49/19.4 75) Inventors: Gregor Fels; Gerhard Ewald, both of 4,981,535 l/1991 Hadermann et al. .................. 149/19.2 Haltern, Germany 4,983.235 l/1991 Nyqvist et al. .. 149/109.6 5,057,553 10/1991 Zagefka et al. ........................, 523/80 73) Assignee: Wasagchemie Sythen GmbH, Haltern, 5,114,630 5/1992 Newman et al. ..... 264/3.4X 5,250,687 10/1993 Lukasavage et al. ................... 544/215 Germany 5,354,520 10/1994 Oliver et al....... ... 264/3.4 X 5,395,559 3/1995 Kaldas et al. ........................ 264/3.4X 21 Appl. No.:759,987 FOREIGN PATENT DOCUMENTS 22 Filed: Dec. 3, 1996 733552 3/1943 Germany. Related U.S. Application Data 1 072 169 12/1959 Germany. 1944 459 3/1971 Germany. 2 336 004 2/1975 Germany. 62) Division of Ser. No. 204,323, Mar. 7, 1994, Pat No. 2 335 251 2/1977 Germany. 5,623,168. 3 617 408 6/1987 Germany. 30 Foreign Application Priority Data 4012 417 10/1991 Germany. 473 057 11/1937 United Kingdom. Sep. 18, 1991 DE Germany .......................... 41 31 O72. Jan. 14, 1992 DEl Germany .......................... 4200 743.7 OTHER PUBLICATIONS (51) Int. Cl. ................ F42B 4/00; C06B 21/00 Verfahren zur Kristallisation aus Lösungen, Dietrich 52 U.S. Cl. ............................. 86/21; 86/20.12; 264/3.4: Schliephake, Chem-Ing-Tech 52, (1980) Nr. 7, S.553-561. 264/3.6; 149/109.6 Primary Examiner-Peter A. Nelson 58 Field of Search ..................... 86/20.12, 21; 264/3.4, Attorney, Agent, or Firm-Bell, Seltzer, Park & Gibson. 264/3.5.3.6; 149/109.6 P.A. 56 References Cited 57 ABSTRACT U.S. PATENT DOCUMENTS A method and an apparatus for reducing the grain size of 1,801,509 4/1931 Jackman .................................. 564/107 crystalline explosive provide for, first of all, dissolving the 2,204,059 6/1940 Acken ..... ... 558/485 coarse crystalline explosive in an organic solvent. 2,346,116 4/1944 Snelling ............. ... 14.9/13 Subsequently, the dissolved explosive is brought together 2,421,778 6/1947 Fleischer et al. ... 149/26 with ice water in a precipitation reactor. In the precipitation 2,867.647 1/1959 Gow et al. ..... ... 149/11 reactor the precipitation and crystallization of the explosive 2,938.233 5/1960 Nack et al. ..... ... 18/47.2 3,173,818 3/1965 Holloway et al. ... 49/35 occur, while turbulent agitation takes place. Afiltration stage 3,635,835 l/1972 Peterson ................. ... 252/35 is connected downstream of the precipitation reactor. A fine 3,702,353 11/1972 Henderson et al. ... ... 264/3.5 crystalline explosive is obtained, having a mean particle size 3,952,655 4/1976 Kusakabe et al. ..... ... 102,312 of from 4 to 6 micrometers. 3,954,526 5/1976 Mangum et al. .. ... 149/7 4,088,518 5/1978 Kehren et al. ............................ 149/11 5 Claims, 1 Drawing Sheet U.S. Patent Oct. 28, 1997 5,682,004 -51 23 24 K () 25 D 14 18 27 X-19 20 O (O 2 22 32 30 33 s 3 44 40 l 4 45 5,682,004 1 2 APPARATUS FOR REDUCTION OF THE to the solvent container and a second return conduit for the GRANSIZE OF CRYSTALLINE EXPLOSIVE accumulated water leads to the ice water container. The method according to the invention provides for the CROSS REFERENCE TO RELATED explosive solution to be brought together with cold water. APPLICATION Under turbulent agitation, the precipitation and crystalliza tion of the explosive take place. The explosive is yielded in This application is a division of application Ser. No. fine crystalline form. In the case of hexogen, mean grain 08/204323, filed Mar. 7, 1994, now U.S. Pat. No. 5,623,168. sizes of from 4 to 6 micrometers can be obtained by the BACKGROUND OF THE INVENTION method according to the invention. The resulting final O product, which still needs to be separated from solvent and The invention relates to a method of and an apparatus for water after crystallization, is characterized by great handling reducing the grain size of crystalline explosive, especially safety. The method according to the invention, furthermore. hexogen or mixtures containing hexogen, wherein the explo offers a high degree of safety in application. sive is dissolved in an organic solvent, the dissolved explo According to a further development of the invention the sive subsequently is precipitated and crystallized in the 15 cold water has a temperature of below 3° C. Conveniently, presence of water, and then the resulting recrystallized ice water is used for this purpose which is prepared in a explosive is separated from solvent and water. separate ice water container. Also the vessel in which In the context of the present application, crystalline precipitation and crystallization take place is cooled advan explosive, in the first place, is understood to be hexogen tageously. (RDX), also octogen (HMX) and nitropenta (PETN), but 20 The method according to the invention readily can be also any other explosive which is available in crystalline carried out continuously in a reactor, in accordance with form as well as mixtures of such explosives. claim 3. The final product in the preparation of hexogen and other A particularly important further development of the crystalline explosives is obtained in coarse crystalline form. invention resides in the addition of a precipitant for precipi 25 tation of the explosive which precipitant retards crystal For many cases of application, however, the crystalline growth. In this manner an explosive of especially small explosive is required to be infine crystalline form, especially particle size is obtained from the crystallization. A decom if it is a constituent of a propellant charge powder. position product of starch, preferably dextrin is used to In the case of a known method of reducing the grain size, advantage as the precipitant. Yet derivatives of starch or the crystalline explosive is ground in a mill while liquid is cellulose which are soluble in water and/or greatly diluted being added. The mechanical crushing of the violent explo solutions of different sugars also may be used as precipitat sive is to be classified as dangerous in spite of the addition ing agent. The addition of the precipitant advantageously of liquid. Moreover, with the known method, the separation occurs at a concentration of from 0.1 to 3% by weight, of the fine fraction can be accomplished with difficulty only. preferably from 0.5 to 1% by weight, based on the explosive Amethod of the kind mentioned initially is already known 35 used. The precipitant advantageously is fed to a precipitation from European patent application 0 340 188 by means of reactor together with the cold water or ice water, with which the average grain size of hexogen and other crystal dissolved explosive being added to the same as well. The line explosives can be reduced to a mean particle size of less precipitant retards or impedes crystal growth and leads to than 20 micrometers. With the known method, the more uniformly rounded crystals. Especially the use of explosive, such as hexogen is dissolved in a solvent and dextrin proved to be advantageous since the addition of water at a temperature between 60° C. and 70° C. and while dextrin has a phlegmatizing effect in that it greatly reduces being stirred. The explosive solution is conveyed into a or totally eliminates the static charging of the dry explosive steam ejector, while being pressurized by nitrogen. In the and, moreover, reduces the sensitivity to friction of the ejector, crystallization takes place, the solvent evaporating explosive. It is preferred to use a white dextrin. White and the explosive precipitating. The precipitated crystalline 45 dextrins are closely related to starch when it comes to their explosive then is separated in a downstream cyclone. A characteristics. They consist predominantly of shortened mean particle size of 8 micrometers is said to be obtainable molecule chains with little branching and can be dissolved by the known process. quickly in water without lumping. It is the object of the invention to propose a method and For best exploitation of the solvent used, it is advanta an apparatus by means of which very small grain sizes can 50 geous if the dissolution of the explosive takes place at a be obtained and with which a very high degree of safety in temperature which is just below the boiling point of the application is achieved. solvent. Ketones, preferably almost anhydrous acetone, can be used to advantage as solvents. When using acetone, the SUMMARY OF THE INVENTION optimum ratio between the acetone used and the water used The above and other objects of the invention are achieved 55 is approximately 30/70. If the amount of water is less, the by the provision of an apparatus which comprises a reactor, crystallization may suffer. Greater quantities of water are a cooling means and an agitator associated with the reactor, possible, yet they render the recovery of the acetone by a solvent container for dissolving the explosive connected distillation unnecessarily uneconomical. upstream of the reactor and provided with a heater means In further modifying the invention, it is provided to filter and an agitator, and an ice water container for making cold the resulting mixture of explosive, solvent, and water so as water connected upstream of the reactor and provided with to separate the precipitated explosive.
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