I was asked to join and post on my experiments so here they are, I apologise for the not too detailed post, but my personal life fucked up so I couldnt type too much.
Here is the thread I promised on energetic materials. Here I will give a few synth's I use in my lab for energetic compounds.
Firstly, why not the Secondary high explosive Nitromannite or Mannitol Hexanitrate. This explosive is interesting as it can low-order detonate from the flame of match but not the spit of fuse.
Properly pressed, its VoD is about 8000m/s and it has positive oxygen balance.
Synthises:
Cool 6.5ml of 96% or higher concentrated H2SO4 (sulphuric acid) in a beaker to below 0 degrees Celcius.
To this add 9.5 grams finely powdered, pure, dry Ammonium Nitrate (NH4NO3) and stir like a madman until it is all dissolved. Then cool to -5 degrees Celcius.
Place the acid/nitrate mix in an ice bath.
Slowly add, in 100mg amounts, 1 gram pure, dry powdered Mannitol to the beaker with stirring, keeping temp below 0 degrees celcius.
When addition is finished, leave for 5 minutes or so add 5.5ml more H2SO4 keeping temp sub zero.
Allow to stand for 5 minutes.
Dump into 100ml ice water. Some use 1 litre, I use down to 50ml on occasion.
Filter and neutralize with bicarb solution, wash, dry. You can re-crystallize from EtOH but if its denatured with pyridine DONT. Beilstein says pyridine in EtOH destroys MHN.
'Store in a cool, dark, dry place away from children, kewls and animals'.
MHN is a EXCELLENT base charge in caps. You can scale that synth up as much as you wish. I sometimes get only 0.5g MHN per 1g Mannitol, but hell, its the OTC method so yield dont matter, and you can increase yield with practise, varying the temp and such. I save my 98% HNO3 for RDX production.
Now lets look into ETN using a variant of Azidechem's method...
175ml 96% H2SO4 is chilled to below zero degrees celcius in an ice bath.
240 grams NH4NO3 is added in portions with vigorous stirring until all dissolved, temp kept below 10 degrees celcius.
The mix is cooled again to below zero.
75 grams erythritol is added in portions keeping temp between 10 degrees and 15 degrees.
Stir like crazy during the additions.
Stir for 15 mins after the additions.
With vigorous stirring 330ml 96% H2SO4 is added keeping temp below 15 degrees.
Stir like mad allowing to react for 15 mins.
Crash into 3 litres of icewater and filter.
Neutralize with bicarb.
Recrystallize from hot bicarb acetone then from methanol.
Wash in water until its neutral and not smelling of MeOH or acetone.
Recrystallization is highly important, to make the ETN stable. ETN is good explosive, castable and 8000m/s VoD when well pressed. Yield about 115-125 grams.
My next post will discuss primary high explosives.
Here is the thread I promised on energetic materials. Here I will give a few synth's I use in my lab for energetic compounds.
Firstly, why not the Secondary high explosive Nitromannite or Mannitol Hexanitrate. This explosive is interesting as it can low-order detonate from the flame of match but not the spit of fuse.
Properly pressed, its VoD is about 8000m/s and it has positive oxygen balance.
Synthises:
Cool 6.5ml of 96% or higher concentrated H2SO4 (sulphuric acid) in a beaker to below 0 degrees Celcius.
To this add 9.5 grams finely powdered, pure, dry Ammonium Nitrate (NH4NO3) and stir like a madman until it is all dissolved. Then cool to -5 degrees Celcius.
Place the acid/nitrate mix in an ice bath.
Slowly add, in 100mg amounts, 1 gram pure, dry powdered Mannitol to the beaker with stirring, keeping temp below 0 degrees celcius.
When addition is finished, leave for 5 minutes or so add 5.5ml more H2SO4 keeping temp sub zero.
Allow to stand for 5 minutes.
Dump into 100ml ice water. Some use 1 litre, I use down to 50ml on occasion.
Filter and neutralize with bicarb solution, wash, dry. You can re-crystallize from EtOH but if its denatured with pyridine DONT. Beilstein says pyridine in EtOH destroys MHN.
'Store in a cool, dark, dry place away from children, kewls and animals'.
MHN is a EXCELLENT base charge in caps. You can scale that synth up as much as you wish. I sometimes get only 0.5g MHN per 1g Mannitol, but hell, its the OTC method so yield dont matter, and you can increase yield with practise, varying the temp and such. I save my 98% HNO3 for RDX production.
Now lets look into ETN using a variant of Azidechem's method...
175ml 96% H2SO4 is chilled to below zero degrees celcius in an ice bath.
240 grams NH4NO3 is added in portions with vigorous stirring until all dissolved, temp kept below 10 degrees celcius.
The mix is cooled again to below zero.
75 grams erythritol is added in portions keeping temp between 10 degrees and 15 degrees.
Stir like crazy during the additions.
Stir for 15 mins after the additions.
With vigorous stirring 330ml 96% H2SO4 is added keeping temp below 15 degrees.
Stir like mad allowing to react for 15 mins.
Crash into 3 litres of icewater and filter.
Neutralize with bicarb.
Recrystallize from hot bicarb acetone then from methanol.
Wash in water until its neutral and not smelling of MeOH or acetone.
Recrystallization is highly important, to make the ETN stable. ETN is good explosive, castable and 8000m/s VoD when well pressed. Yield about 115-125 grams.
My next post will discuss primary high explosives.