BTNEC

     BTNEC, an acronym for Bis(2,2,2 trinitroethyl) carbonate, is a high explosive sometimes used in smokeless propellant and liquid explosive formulations. Other names for BTNEC include 2,2,2-trinitroethanol carbonate ester; and bis(2,2,2-trinitroethyl) ester carbonic acid. BTNEC is unique an important because of its very high oxygen content per cc; it is even greater than liquid oxygen itself. BTNEC is especially useful in compositions along with metallic components because of its oxygen content. It is often combined with aluminum powder, and it forms melt castable explosives with RDX and picric acid. BTNEC is more powerful than either RDX or TNT, while at the same time having similar stability. It can be used alone in admixture with 5-10% wax as a desensitizer.

CHEMICALS	APPARATUS
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     Synthesis 1: Prepare a solution of 9.9 g of phosgene and 250 mL of tetrachloromethane in a 500-mL round-bottom flask. Cool the solution by immersing in an ice bath. Add 40 g of 2,2,2-trinitroethanol to the solution with swirling. After all of the trinitroethanol has dissolved add 6.5 g of granular anhydrous aluminum chloride. Set up the flask for refluxing and heat it to 40 C using ice cold water to condense the tetrachloromethane and phosgene vapors. A considerable quantity of hydrogen chloride vapors will be released during the reaction, so a well ventilated area is necessary. Once the reaction has started, as observed by hydrogen chloride emission, add an additional 6.5 g of aluminum chloride and continue heating at 40 C for 3 hours. After this time slowly warm the flask over a period of 1 hour to a warmer reflux temperature, and then hold at that temperature for 1 hour. The reaction mixture is allowed to cool and nitrogen gas is bubbled into the flask to remove any remaining hydrogen chloride vapors. Dilute the flask with hexane and cool to -20 C. A gummy solid precipitate should form, which can be filtered to collect it. The solid is dissolved in dilute hydrochloric acid, added to a separatory funnel, and extracted with a portion of chloroform. The solvent filtrate portion can be gently heated to evaporate the trichloromethane, upon which an oil is obtained. Add a small portion of chloroform to this oil and add the previous chloroform extract. The solution is added to a separatory funnel, washed with a few portions of water, and allowed to evaporate upon which a crude crystalline material is obtained. This material can be purified by recrystallization from chloroform. The final yield of purified BTNEC is about 4 g. Alternatively you can prepare BTNEC by combining 18.1 g of trinitroethanol, 6.7 g of powdered aluminum chloride, and 40 mL of liquid phosgene in a stainless steel pressure reactor. The reactor is sealed, gradually heated to room temperature, shaken several times, and heated to 50 C and held at that temperature for 19 hours. The vessel is cooled, opened to vent unreacted phosgene, and the contents added to a flask along with 200 mL of carbon tetrachloride and 18.1 g of trinitroethanol. The flask is refluxed for 8 hours at 76 C, cooled in ice to precipitate some product, and the product filtered to collect it. The solid can be recrystallized from a mixture of chloroform and hexane to obtain a batch of BTNEC, about 11 g. The liquid filtrate can supply additional product by dilution with ether, and washing in a separatory funnel with water and sodium bicarbonate solution. The washed solvent is gently heated to evaporate it and an additional crop of BTENC will form. After recrystallization it can yield another 10 g. Synthesis 2: In a 50-mL beaker prepare a mixture of 10 g of 2,2,2-trinitroethanol and 5.25 g of pyridine N-oxide in 6 mL of methylene chloride and 13 mL of chloroform. Phosgene gas is bubbled into the beaker at a rate of 18 cc per minute for 90 minutes while the temperature is maintained at 25 C. The mixture is then stirred for 60 minutes and poured into a 100-mL beaker with 50 mL of n-hexane while stirring. A precipitate should form. After settling, the hexane is decanted off, and 50 g of ice is added. When the ice melts the product is collected by filtering, washed with water, and allowed to dry. Yield of BTNEC is about 76%. One example of a mixture containing BTNEC in an explosive formulation used in missile warheads is as follows: Blend together 31% BTNEC, 10% trinitrobenzene, 22% RDX, 31% aluminum powder, and 6% wax. Another formulation used in underwater blasting is as follows: Combine 26% BTNEC, 10% trinitrobenzene, 22% RDX, 37% aluminum, and 5% wax.

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