Benn
October 23rd, 2006, 04:15 PM
Hi all, i`ve read a lot about interested explosives like ethylene glycol dinitrate (EGDN), diethylene glycol dinitrate (DEGDN) and triethylene glycol dinitrate (TEGDN). I have been thinking that this is suitable to prepare triethanolamintrinitrate by several methods, it is a nitrated ester and the synthesis is somewhat sensitive when the temperature is not maintained exactly.
Triethanolaminetrinitrate: (O2NOCH2CH2)3N
284,18 g/mol
Synthesis 1:
Prepare a mixture of 55 g of 96% sulfuric acid and 33,5 g of 70% nitric acid in a 500 mL round bottomed flask and cool the flask to 0 degree centigrade. Prepare solution of 100 mL of methylene chloride and 12,5 mL of triethanolamin in a 250 mL round bottomed flask and cool the solution much as possible, the triethanolamin in the solution should not freeze.
Triethanolamine: (HOCH2CH2)3N
Freezing-point: 17,9 - 21 degree centigrade
Molar Mass: 149,19 g/mol
Density: 1,12 g/cm³
Boiling Point: ~360 degree centigrade
CAS number: 102-71-6
Slowly the second solution is stirred to the first, keep the temperature between 0 and 2 degree centigrade and the mixture is stirred for 15 minutes. After that, allow the layers to separate and the uppler layer is tranfered to a separatory funnel. Wash the solution with four 30 mL portions of water, let separate the layer and wash the TEATN with a portion of 10% sodium carbonate solution. The solvent can be removed by gently warming the flask on a water bath at 50 degree centigrade.
Synthesis 2:
Prepare a mixture of 100 g of 98-100% sulfuric acid, 172 g of 98-100% nitric acid and 667 mL methylene chloride in a large round bottomed flask and cool the flask to 0 degree centigrade. Prepare solution of 200 mL of methylene chloride and 99,5 g of triethanolamine in a 500 mL round bottomed flask and slowly the triethanolamine solution is stirred to the acid mixture. Hold the temperature between 0 and 2 degree centigrade and the stirring is continued for 15 minutes. Add 16 mL of water and let separate the layers. Decant of the upper layer, transfer the solution to a separatory funnel, wash the product with four 200 mL portions of water, separate the product and wash with one portion of 10% sodium carbonate solution. The solvent is than removed by gently warming the flask on a water bath at 50 degree centigrade.
Synthesis 3:
Prepare 2,2 mL of a nitrating mixture consisting of 51% sulfuric acid and 49% nitric acid in a 100 mL beaker by cooling the beaker to 0 degree centigrade in a salt ice bad. Careful add 107 mL of n-heptane to the beaker and keep the temperature below 2 degree centigrade. Slowly add 1 mL of triethanolamine with stirring, stirr the mixture for additional 15 mintues and keep the temperature between 0 and 2 degree centigrade. After stirring three layers should form in the beaker. Tranfer the layers to a separatory funnel, allow the layers to form and collect the middle layer of TEATN. Wash with four small portions of water, let separate the layer and wash again with a small portion of 10% sodium carbonate solution. The solvent is than removed by gently warming the flask on a water bath at 50 degree centigrade.
Does anyone have any experience making this explosive ?
Triethanolaminetrinitrate: (O2NOCH2CH2)3N
284,18 g/mol
Synthesis 1:
Prepare a mixture of 55 g of 96% sulfuric acid and 33,5 g of 70% nitric acid in a 500 mL round bottomed flask and cool the flask to 0 degree centigrade. Prepare solution of 100 mL of methylene chloride and 12,5 mL of triethanolamin in a 250 mL round bottomed flask and cool the solution much as possible, the triethanolamin in the solution should not freeze.
Triethanolamine: (HOCH2CH2)3N
Freezing-point: 17,9 - 21 degree centigrade
Molar Mass: 149,19 g/mol
Density: 1,12 g/cm³
Boiling Point: ~360 degree centigrade
CAS number: 102-71-6
Slowly the second solution is stirred to the first, keep the temperature between 0 and 2 degree centigrade and the mixture is stirred for 15 minutes. After that, allow the layers to separate and the uppler layer is tranfered to a separatory funnel. Wash the solution with four 30 mL portions of water, let separate the layer and wash the TEATN with a portion of 10% sodium carbonate solution. The solvent can be removed by gently warming the flask on a water bath at 50 degree centigrade.
Synthesis 2:
Prepare a mixture of 100 g of 98-100% sulfuric acid, 172 g of 98-100% nitric acid and 667 mL methylene chloride in a large round bottomed flask and cool the flask to 0 degree centigrade. Prepare solution of 200 mL of methylene chloride and 99,5 g of triethanolamine in a 500 mL round bottomed flask and slowly the triethanolamine solution is stirred to the acid mixture. Hold the temperature between 0 and 2 degree centigrade and the stirring is continued for 15 minutes. Add 16 mL of water and let separate the layers. Decant of the upper layer, transfer the solution to a separatory funnel, wash the product with four 200 mL portions of water, separate the product and wash with one portion of 10% sodium carbonate solution. The solvent is than removed by gently warming the flask on a water bath at 50 degree centigrade.
Synthesis 3:
Prepare 2,2 mL of a nitrating mixture consisting of 51% sulfuric acid and 49% nitric acid in a 100 mL beaker by cooling the beaker to 0 degree centigrade in a salt ice bad. Careful add 107 mL of n-heptane to the beaker and keep the temperature below 2 degree centigrade. Slowly add 1 mL of triethanolamine with stirring, stirr the mixture for additional 15 mintues and keep the temperature between 0 and 2 degree centigrade. After stirring three layers should form in the beaker. Tranfer the layers to a separatory funnel, allow the layers to form and collect the middle layer of TEATN. Wash with four small portions of water, let separate the layer and wash again with a small portion of 10% sodium carbonate solution. The solvent is than removed by gently warming the flask on a water bath at 50 degree centigrade.
Does anyone have any experience making this explosive ?