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The Preparatory Manual of Explosives: The Revision: A comprehensive Encyclopedia of laboratory processes for the preparation of highly energetic materials
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- Mã sản phẩm: B08F6Y555S
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- ASIN:B08F6Y555S
- Publisher:Independently published (August 6, 2020)
- Language:English
- Paperback:683 pages
- ISBN-13:979-8672973647
- Item Weight:4.11 pounds
- Dimensions:8.27 x 1.71 x 11.69 inches
- Best Sellers Rank:#948,159 in Books (See Top 100 in Books) #797 in Education Research (Books) #10,037 in Encyclopedias & Subject Guides
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From the Publisher
Preparation of dinitrotoluenes
Into a suitable sized 3-neck flask, equipped with mechanical stirrer, thermometer, and addition funnel, and sitting inside a round bottom heating mantle, pour in 382 grams of 70% nitric acid, and then slowly and carefully add in 789 grams of 98% sulfuric acid. Thereafter, pour the collected liquid layer heated to 45 Celsius (the mononitrotoluenes) from step 1, into the addition funnel (keep heated at 45 Celsius), and then turn on the heating mantle and heat the nitrating acid mixture to 74 Celsius (approximate). When the nitrating acid mixtures temperature reaches 74 Celsius, begin stirring the nitrating acid mixture and then slowly drip in the collected liquid layer heated to 45 Celsius (the mononitrotoluenes) from step 1 from the addition funnel into the nitrating acid mixture, while rapidly stirring the nitrating acid mixture. Note: during the addition of the mononitrotoluenes heated liquid product from the addition funnel, the temperature of the nitrating acid mixture will begin to rise, so do not increase any temperature using the heating mantle. Carefully drip in the heated mononitrotoluenes from the addition funnel to the nitrating acid mixture,but monitor the temperature of the nitrating acid mixture and do not allow it to rise above 85 Celsius. During the addition of the heated liquid mononitrotoluenes from the addition funnel into the nitrating acid reaction mixture, continue to rapidly stir the nitrating acid mixture. After the addition of the mononitrotoluenes from the addition funnel is complete, continue to rapidly stir the reaction mixture and allow its temperature (around 85 Celsius) to slowly drop back down to 74 Celsius under rapid stirring, and hold this temperature under stirring for about 1 hour. Thereafter, while the reaction mixture is still hot (around 74 Celsius), quickly pour this hot reaction mixture into a clean large separatory funnel, and then allow the reaction mixture to stand in the separatory for a few minutes, and then immediately thereafter, drain-off the bottom acid layer, and then collect the upper oily hot liquid dinitrotoluenes layer. Once this upper hot liquid layer has been collected, pour it into a clean beaker, sitting on top of a hot plate, and equipped with mechanical stirrer, and keep this collected liquid layer heated to 74 Celsius under moderate stirring until use for step 3. Note: if this collected hot oily liquid layer cools below 70 Celsius, the 2,4-dinitro, 2,6-dinitro, and 2,3-dinitro isomers will crystallize, and the entire layer will solidify, so this heated product should be used as soon as possible in step 3.
Ammonium Nitrate Dynamite (AND) or Ammonia Dynamite (Ammondynamit, in German)
A type of “straight” (powdery) dynamite in which up to 50% of liquid nitric ester (nitroglycerine or nitroglycerine + antifreeze additives) is replaced by ammonium nitrate and the remaining nitric ester acts as a sensitizer for the insensitive ammonium nitrate. These explosives, which originated in the USA about 50 years ago are notable for their heaving rather than shattering effect and their strength is lower than that of “straight” dynamites. Ammonium Nitrate Dynamite’s (AND’s) have been used for blasting soft rocks, clays and for earth excavations. They are not suitable, however, for use in coal mining except “strip-mining”, called “open-cast mining” by the British. Ammonium Nitrate Dynamite’s were also used in some European countries and compositions and properties of some of these Ammonium Nitrate Dynamite’s are given in the following tables. Some Ammonium Nitrate Dynamite’s were used for military purposes, such as demolition, excavation and cratering work. DuPont Co., Wilmington, Delaware has been manufacturing several brands of ammonia dynamites, such as “DuPont Extra”, “Red Cross Extra”, “Red Cross Blasting FR” etc. Some of their properties are given in reference 8, but their composition seems to be a trade secret. According to Stettbacher (see reference 7), the German ammonium nitrate explosives containing more than 4% of nitroglycerine were not considered as safe for use in coalmines. The name “Ammonsalpetersprengstoffe” was applied only to ammonium nitrate explosives containing not more than 4% nitroglycerine.
HMX. Octogen; CYCLOTETRAMETHYLENETETRANITRAMINE
Molecular Info: Molecular Formula = C4H8N8O8; Formula Weight = 296.15512; Composition = Carbon content (16.22%) Hydrogen content (2.72%) Nitrogen content (37.84%) Oxygen content (43.22%); Molar Refractivity = 58.20 ± 0.4 cm3 ; Molar Volume = 151.7 ± 5.0 cm3 ; Parachor = 501.2 ± 6.0 cm3 ; Index of Refraction = 1.693 ± 0.03; Surface Tension = 119.0 ± 5.0 dyne/cm; Density = 1.95 ± 0.1 g/cm3 ; Polarizability = 23.07 ± 0.5 10-24cm3 ; Monoisotopic Mass = 296.046509 Da; Nominal Mass = 296 Da; Average Mass = 296.1551 Da; M+ = 296.045961 Da; M- = 296.047058 Da; [M+H]+ = 297.053786 Da; [M+H]- = 297.054883 Da; [M-H]+ = 295.038136 Da; [M-H]- = 295.039233 Da. [Called in Great Britain HMX (High Melting Explosive of His Majesty's Explosive), in France Cyclotetramehylene-tetranitramine or Octogene, in Germany Octogen and in Russia Oktoghen]. Forms white crystals (from nitromethane), melting point: 276-280 Celsius with decomposition), density: 1.90, soluble in solvents which dissolve RDX (qv); insoluble in water & non-hygroscopic. HMX is formed under some conditions, in the nitration of hexamethylene-tetramine, hence it is present in Type B RDX. Preparation (see reference 7). In the first stage, hexamine, glacial acetic acid, acetic anhydride, AN & HNO3 are added simultaneously, continuously & equivalently and the temperature is maintained at 45 Celsius. The reaction mixture is aged 15 minutes. The second stage reactants: AN/HNO3 /acetic anhydride are added over a 25-minute period and aged 65 minutes. The mixture is poured into water and simmered on a steam bath for 12 hours. The precipitate of RDX-HMX contains 73% of HMX. The RDX is destroyed, leaving HMX, by placing the crude product in a solution of sodium tetraborate decahydrate in water, heating to boiling, and adding 5N NaOH. When the pH increases from 8.7 to over 9.7, complete destruction of the RDX has taken place. The HMX is filtered from the hot mixture & recrystallized from nitromethane. This is the beta form of HMX. The present method of preparing HMX is essentially that of earlier workers (see references 2, 6, 7, 10, 11, 12, 13, 14, 16 & 23), however, it is somewhat refined and paraformaldehyde is added to increase the yield (see reference 18). Procedure: To a 6 to 10-liter flask equipped with stirrer, thermometer & 3 dropping funnels, add 785 grams of acetic acid, 13 grams of acetic anhydride & 17 grams of paraformaldehyde while maintaining the temperature at 44 ± 1 Celsius with a water bath. Add over a 15 minute period, with constant stirring, a solution of 101 grams of hexamine in 165 grams of acetic acid, 320 grams of acetic anhydride & 180 grams of HNO3- AN solution (prepared by dissolving 840 grams of AN in 900 grams of HNO3, 99% or stronger). The hexamine & HNO3 are added continuously and proportionally. The mixture is aged for 15 minutes. Then add 320 grams of acetic anhydride & 271 of HNO3-AN solution proportionately, and then 160 grams of acetic anhydride in bulk. Allow the mixture to age for 60 minutes and reflux for 30 minutes after adding 350 grams of hot water. Cool to 20 Celsius by adding ice, collect the water-insoluble precipitate and wash with 3 portions of cold water. The yield of 200 grams HMX is 95% of theory and the purity is higher than 90%. This product is alpha-HMX which is converted to beta form by crystallization from boiling acetone, acetonitrile or cyclohexanone using equal parts by weight of solid & solvent. The recrystallized HMX has a melting point of 278-279 Celsius. Polymorphs. HMX exists in 4 polymorphic modifications between room temperatures & its melting point (280 Celsius). These polymorphs are known as alpha, beta, gamma & delta forms. With each polymorph, there is associated a stability range, and differences in physical props such as density, solubility & refractive indices. These polymorphs can also undergo transformations. The common modification of HMX is the beta form. Therefore, when the unqualified term HMX is used, it is understood to be the beta form. This modification is prepared by the very slow cooling of solutions of HMX in acetic acid, acetone, nitric acid or nitromethane. The crystals formed are monoclinic with a density of 1.90 g/ml. Alpha HMX can be prepared by crystallizing from the same solvents as used in the preparation of beta-HMX, except that the solutions must be cooled rapidly. Its crystalline form is orthorhombic with a density of 1.82 g/ml. Gamma-HMX is prepared from the same solvents as alpha & beta forms but with much more rapid cooling. The crystals are monoclinic with a density of 1.76 grams/ml. Delta-HMX can be crystallized most readily from solvents in which it is only slightly soluble, such as acetic acid or tris(beta-chloroethyl) phosphate, and rapid chilling, preferably in small amts poured over ice. The crystals are hexagonal with a density of 1.80 grams/ml. The polymorphs of HMX may be obtained also by heating, for example, beta-HMX is converted to alpha above 102-104.5 Celsius; alpha to gamma above 160-164 Celsius, gamma is meta-stable to 160-164 Celsius; and above 160- 164 Celsius to melting point delta is formed. However, these values are controversial (See references 15 & 28). More detailed info on the preparation of HMX polymorphs is given in references 5, 29 & 30. The order of sensitivity of the polymorphs of HMX may be summarized as follows: delta >gamma> alpha> beta. The range of values obtained using an Explosives Research Laboratory, Bruceton, Pa Apparatus (Type' 12) with a 2.5 kg weight is as follows: delta 19.2, gamma 13.8 to 33.9, alpha 15.6 to 26.4, and beta 21.2 to 24.9cm. A value of 12cm for PETN was obtained under the same conditions (see reference 28).
Preparation of TATB
Step 1: Preparation of 3,5-dichloro-anisole Into a 3-neck flask, equipped with mechanical stirrer, thermometer, and wide mouth funnel, and said 3-neck flask sitting inside a round bottom heating mantle, pour into the 3-neck flask 500 milliliters of pre-heated DMSO (25 Celsius), and then add in all at once, 100 grams of 1,3,5-trichlorobenzene. Thereafter, turn on the stirrer to high speed, and then turn on the heating mantle to 62 Celsius. When the reaction mixture has reached 62 Celsius, slowly add in, in small portions at a time, 36 grams of sodium methoxide over a period of about 30 minutes, while continuing to rapidly stir the reaction mixture and maintain its temperature at 62 Celsius. Once all the sodium methoxide has been added, continue to heat the reaction mixture at 60 to 62 Celsius for about 8 hours. After 8 hours, turn off the heating mantle, and allow the reaction mixture to cool to room temperature; during the cool down period, continue to rapidly stir the reaction mixture. Once the reaction mixture has cooled to room temperature, disassemble the apparatus, and then drown the entire reaction mixture into 2000 milliliters of ice water, and then mechanically stir this mixture for 45 minutes. After 45 minutes, filter-off the desired precipitated product using a clean Buchner funnel under moderate suction, wash with six 150-milliliter portions of ice-cold water, and then suction dry as best as possible. Finally, recover the suction dried product from the Buchner funnel, and place onto a shallow pan or tray, and allow it to thoroughly air dry. Once dry, collect the dried product, crush into a powder, and then save for step 2. Step 2: Preparation of 3,5-dichloro-2,4,6-trinitroanisole Into a 3-neck flask, equipped with mechanical stirrer, thermometer, and wide mouth funnel, and said 3-neck flask sitting inside an ice/salt bath, pour into the 3- neck flask 100 milliliters of 90% nitric acid, and then slowly and carefully add in 230 milliliters of 98% sulfuric acid, and then cool this nitrating acid mixture to 0 Celsius. When the nitrating acid mixture chills to around 0 Celsius, slowly add in, in small portions at time, 71 grams of 3,5-dichloroanisole (prepared in step 1) over a period of 15 minutes while stirring the nitrating acid reaction mixture, and maintaining its temperature below 55 Celsius at all times. Note: during the reaction, the temperature of the reaction mixture will rise to 50 Celsius. After addition of the 3,5-dichloroanisole, replace the now depleted salt/ice bath, with a fresh ice/salt bath, and cool the reaction mixture to 0 Celsius with stirring, and stir and cool at 0 Celsius for about 45 minutes. After 45 minutes, remove the cooling bath, and allow the reaction mixture to warm to room temperature; during such time, continue to rapidly stir the reaction mixture. Thereafter, place the 3-neck flask into a round bottom heating mantle, replace the wide mouth funnel with a bulb reflux condenser, and then turn on the heating mantle to 100 Celsius, and then heat and rapidly stir the reaction mixture at 100 Celsius for 45 minutes. After 45 minutes, remove the heat source, and allow the reaction mixture to cool to room temperature; during the cool down period, continue to rapidly stir the reaction mixture. Thereafter, disassemble the apparatus, and then carefully and slowly pour the entire reaction mixture onto 1 kilogram of ice contained in a suitable sized beaker, allow the ice to melt, and then mechanically stir this diluted mixture for 45 minutes. Thereafter, filter-off the precipitated product using a clean Buchner funnel, under moderate suction, wash with six 150-milliliter portions of 10% sodium carbonate solution, followed by six 350-milliliter portions of warm water, and then suction dry as best as possible. Finally, recover the suction dried product from the Buchner funnel, and place onto a shallow pan or tray, and allow it to thoroughly air dry. Once dry, collect the dried product, crush into a powder, and then save for step 3. Note: 3,5-dichloro-2,4,6-trinitroanisole is also a high explosive, and can be used as such.
Tetracene. Tetrazene
Molecular Info: Molecular Formula: C2H8N10O2; Formula Weight: 204.15072; Composition: Carbon content (11.77%) Hydrogen content (3.95%) Nitrogen content (68.61%) Oxygen content (15.67%); Molar Refractivity: 41.48 ± 0.5 cm3 ; Molar Volume: 88.8 ± 7.0 cm3 ; Parachor: 317.0 ± 8.0 cm3 ; Index of Refraction: 1.905 ± 0.05; Surface Tension: 162.3 ± 7.0 dyne/cm; Density: 2.29 ± 0.1 g/cm3 ; Polarizability: 16.44 ± 0.5 10-24cm3 ; RDBE: 5; Monoisotopic Mass: 204.08317 Da; Nominal Mass: 204 Da; Average Mass: 204.1507 Da; M+: 204.082621 Da; M-: 204.083718 Da; [M+H]+: 205.090446 Da; [M+H]-: 205.091543 Da; [M-H]+: 203.074796 Da; [M-H]-: 203.075893 Da; Calculated LogP: -1.41+/- 0.74; InChI = 1/C2H7N9O/c3-1(4)6-9-7-2(5)8-10-11- 12/h(H,10,12)(H6,3,4,5,6,7,8,11). Also known as 4-Guanyl-1-(alpha-tetrazol-5-yl)-tetrazene or Guanyldiazo-guanyl Tetrazene. (It must not be confused with naphthacene which is also called Tetracene); (Called Buzylene, rather than Tetrazene, in reference 2, but same structure is meant; in recent literature the term "guanyl" has been replaced by "amidino", and then "carboxamidine"). Patinkin et al (see reference 11) claimed that the Tetrazole Hydrate, rather than the Nitrosaminoguanyl, was the actual structure, but both structures continue in use. Patinkin also prepared a nitrate salt, melting point: 93-94°C (decomposes) of the (claimed) Tetrazole structure but with the 1 and 4 positions of the Tetrazene interchanged. Hofmann et al, the original preparers (see reference 2), also seemed to believe they had the Tetrazole and Nitrosaminoguanyl structure as separate compounds. Its formula given in Davis (see reference 10) and AMCP-706-177. Its hydrate contains 3H2O; OB to CO2 –57.6%, OB to CO ca –43%. A recent study of the structural analysis by single crystal methods (see references 14 & 15) shows that Tetracene is the zwitterion (guanidinium) of 1-Amino-l-[(1H-tetrazole-5-yl)azo-guanidine Hydrate of structure:in contrast to the structure previously assigned by Patinkin et al (see reference 11). Tetracene exists as colorless or pale-yellow needles; melting point: decomposes 142°C and explodes at 160°C in 5 seconds (vs. 190°C for MF); explodes in a flame w/o much noise but producing much black smoke; apparent density only 0.45, but yields a pellet of density 1.05 when compressed at 3,000 psi. It is practically insoluble in water, alcohol, ether, acetone, benzene, CCl4 and ethylene dichloride; soluble in dilute nitric acid; decomposed by boiling water with formation of 2N2 per mole; can easily be dead-pressed (see reference 10). Tetracene was first prepared in 1910 by Hofmann et al (see reference 2) and then studied by them (see reference 3), but the most extensive studies were done by Rinkenbach & Burton (see reference 4) and results of their experiments are given by Davis (see reference 10) and in AMCP 706-177 (see reference 12). Davis (see reference 10, p. 449) describes in detail a method of preparation starting with 35 grams of aminoguanidine bicarbonate, 2500ml distilled water, 15.7 grams of glacial acetic acid and 27.6 grams of Na nitrite. One lab method described in AMCP 706-177 is not in the literature: Tetracene was prepared by dissolving 5 grams of aminoguanidine dinitrate in 30ml of distilled water, cooling to 0°C and mixing with a solution 2.5 grams of Na nitrite in 15ml of water. While maintaining the temp at 10°C, 0.5 grams of glacial acetic acid was added causing precipitation of Tetracene. After allowing the slurry to stand overnight (or longer), the precipitate was washed by decantation with several portions of water and then transferred to filter to be washed more thoroughly with water using suction. Then the product was dried in air at RT and transferred for storage in a bottle provided either with a cork or rubber stopper. Another method of preparation listed in AMCP 706-177 is from aminoguanidine sulfate and Na nitrite in distilled water. Following are explosive properties of Tetracene as given in references: Brisance, by Sand Test. 0.4 grams initiated by No. 6 cap crushed 28.0 grams sand, vs. 23.4 grams by MF or 48.0 grams by TNT; Detonation Rate. not found; Explosion Temperature. 160°C in 5 seconds; Gas Volume. 1,190cc/gram; Heat of Explosion. 658cal/gram; Heat Test at 100°, loss 23.2% in 1st 48 hours, 3.4% in 2nd 48 hours; no explosion in 100 hours; Hygroscopicity. only 0.77% gain at 30°C & RH 90%; Impact Sensitivity, BM App, 2kg weight 7cm, vs. 5cm for MF; Impact Sensitivity. PicArsnApp, 8 oz weight 8 inches, vs. 9-10 inches for MF (Davis, p. 449); Initiating Efficiency, not efficient when used alone for initiating HE's, but is as efficient as MF when initiated externally (Davis, p 450); International Test at 75°C % loss in 48 hours 0.5, vs. 0.18 for MF; Loading, pressed; Power by Trauzl Test. 61% of TNT, vs. 51% by MF; Sensitivity to Electrostatic Discharge, in joules., 0.010 for unconfined and 0.012 for confined; Sensitivity to Initiation, minimum detonating charge 0.40 grams MF; Storage, Wet. Uses: Can be used in detonators when initiated by another primary explosive and functioning as an intermediate booster or when mixed with another primary explosive to increase the sensitivity of the latter to flame or heat. Its mixture with LA was patented by Dynamit AG (see reference 8) for use in explosive rivets. Tetracene can also be used in primer caps where as little as 2% in the composition results in improved uniformity of percussion sensitivity. The following German WWII priming mixtures containing Tetracene are listed in reference 11a, p. Ger 197-L: I. Priming Mixture No. 30/40, used for rifle and pistol cartridges: Tetracene 3, Pb styphnate 40, Ba nitrate 42, Ca silicide 10 & Pb dioxide 5%. II. Duplex-Cap Mixture for use in 20mm & 37mm, as well as in some larger shells, consisted of 0.30 grams of Pb azide 92.5 and Tetracene 7.5% pressed at 100kg/sq-cm over 0.05 grams of un-waxed PETN pressed at 500kg/sq-cm. III.
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