TATB

     TATB, an acronym for 1,3,5-triamino-2,4,6-trinitrobenzene, is a very insensitive and powerful high explosive. Other names include 2,4,6-trinitro-1,3,5-benzenetriamine; sym-triaminotrinitrobenzene; EDC 35; and TATNB. TATB was first prepared in 1888 by the team of Jackson and Wing, but it was not until the 1950’s that it was recognized as an explosive. TATB is classified as a heat resistant explosive and find uses in numerous applications. TATB is the explosive of choice in the all modern thermonuclear warheads, like the W-87 for example; the explosive surrounds a sphere of beryllium (a neutron reflector) that is in turn wrapped around a sphere of plutonium-239 filled with deuterium-tritium gas. TATB is perhaps the most insensitive high explosive of them all. TATB is rather expensive to manufacture, around $200/Kg, but it has been the subject of numerous studies to develop ever cheaper and more efficient routes of synthesis. Lawrence Livermore has developed a process called vicarious nucleophilic substitution that uses surplus uns-dimethylhydrazine (UDMH) rocket propellant from the former Soviet Union, or the process can use surplus ammonium picrate (explosive D) from the US. Using the surplus material is significantly cheaper, but more importantly the raw material for the traditional synthetic route, trichlorobenzene, is only manufactured in China. It does the US no good to depend on a potential enemy nation for its nuclear defense needs.

CHEMICALS	APPARATUS
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     Synthesis 1: Prepare a solution of 315 mL of toluene and 7 mL of water in a 500-mL round-bottomed flask. Add 30 g of wet trichlorotrinitrobenzene to the solution and stir until it dissolves. The next reaction requires a pressure of several atmospheres, while ordinary lab glassware can handle pressure make sure the flask has no chips or scratches that could weaken it. Connect a right angle adapter to the flask and place an inlet tube or bubbler on the adapter such that the end is close to the bottom of the flask. Seal the other end of the adapter with a one-hole stopper and wire it closed so it can not fly off. Into the hole place the tip of a buret with a stopcock. To regulate the pressure of the reaction the stopcock can be opened to relieve pressure. Place a screen or plastic shield around the flask just in case it bursts. Heat the contents of the flask to 145 C under pressure. Begin bubbling ammonia through the inlet tube at a rate of about 3-4 g per hour. Allow the first bit of ammonia to escape to pure the flask of air. Pressurize the flask to just under 3 atm (35-40 psi) and regulate this pressure via the buret. Hold the pressure at 35-40 psi and the temperature at 150 C for 3 hours while stirring and bubbling in the ammonia. The reaction will produce most of its own heat, but some external heating may be needed. The reaction is complete when a large pressure rise is observed, if left unchecked it could rise to around 60 psi. Stop adding ammonia and allow the mixture to cool to 60 C. Vent the pressure to atmospheric and dump the contents of the flask, while stirring rapidly, into a large beaker filled with 500 mL of water. Filter to collect the precipitate of TATB and wash it with 1-2 L of water. Dry the TATB in an oven at 100 C for 16 hours. Synthesis 2: This procedure prepares fine grained TATB crystals. Into a 500-mL beaker dissolve 15.8 g of trichlorotrinitrobenzene in 140 mL of toluene. Prepare a second solution of 1 g of sodium lauryl sulfate (or 1 mL of oleic acid) and 4 mL of 10% polyvinyl alcohol (in water) in 200 mL of water. Add the second solution to the first. Using a bubbler pass a stream of ammonia gas through the mixture for 1 hour while maintaining the temperature between 35 and 40 C with a water bath. During the ammonia addition the mixture should be stirred very rapidly. An overhead stirrer or a drill with a large blade is recommended to ensure high shear mixing. The faster the mixing, the better the emulsion, and the smaller the TATB particles. The TATB crystals will precipitate as the reaction progresses. Filter to collect the TATB and wash it with cold water. Dry as in synthesis 1. Yield is 98%. Synthesis 3: Dissolve 1 g of pentanitroaniline in 100 mL of either methylene chloride, toluene, or xylene. Bubble anhydrous ammonia into the solution to precipitate TATB. Filter to collect the TATB and wash it with cold water. Dry as in synthesis 1. Yield is 100%. This reaction may be scaled up as large as desired. Synthesis 4: This procedure is a more environmentally friendly vicarious nucleophilic substitution method. Prepare a solution of 1 g of picramide and 17.5 mmol of 1,1,1-triethylhydrazinium chloride (or 17.5 mmol trimethylhydrazinium iodide) in 34 mL of dry DMSO. Add 1.89 g of sodium methoxide in one portion and stir the slurry for 16 hours in a dry atmosphere. Pour the reaction mixture into a small beaker containing 25 mL of ice water. Add concentrated hydrochloric acid to the mixture until it reaches a pH of 4. Filter to collect the product, wash it with 20 mL of water and 10 mL of acetone, and allow to dry in an oven at 100 C for several hours. Final yield of TATB is about 1.07 g or 95%. Synthesis 5: This procedure is a more environmentally friendly vicarious nucleophilic substitution method. Prepare a solution of 0.148 g of trinitrobenzene and 5.10 mmol of 1,1,1-triethylhydrazinium chloride (or 5.10 mmol trimethylhydrazinium iodide) in 10 mL of DMSO. Add 0.600 g of sodium methoxide in one portion and stir at room temperature for 20 hours. Pour the reaction mixture into 200 mL of cold 0.12N hydrochloric acid. Filter to collect the precipitate, wash it with water, and allow to dry in the open. Final yield of TATB is 0.16 g or 61%. Synthesis 6: Prepare a solution of 2.0 g of trimethoxytrinitrobenzene in 50 mL of methyl alcohol, and cool this solution to -10 C. With vigorous stirring bubble ammonia gas into the solution for 90 minutes while keeping the temperature at -10 C. At this point stop cooling the reaction mixture, but continue to bubble ammonia gas into it for an additional 90 minutes. The mixture will gradually warm to room temperature. Filter to collect the product, wash it with methyl alcohol, and allow to dry. Final yield of TATB is about 1.65 g or 97%. Synthesis 7: Into a 50-mL round-bottomed flask containing 1.0 g of trimethoxytrinitrobenzene add 25 mL of liquid ammonia. Stir this mixture under reflux (-33 C) for 6 hours. Distill off the ammonia to obtain a solid yellow material. Add 25 mL of DMSO to the flask and place in a sonication bath for one hour. Filter to collect the crystals of product, wash them with 50 mL of methyl alcohol, and allow to dry. Final yield of crude TATB is about 0.80 g or 95%.

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