So you want to make nitroglycerine ...
Okay, let's do it !!
The stuff needed for making some NG:
- 60 ml of >95% H2SO4 (sulfuric acid)
- 40 grams of NH4NO3 (ammonium nitrate)
- 10 milliliter of glycerine (glycerol)
- At least 0.5 kg of ice for cooling
Pics of the precursors are coming up soon. Or whenever I feel to shoot/upload them ...
Note that I work with clean material here, you don't want nasty side-reactions ...
I can not stress this enough:
Because this synthese involves a pretty sensitive high explosive, you must NEVER let temperature rise over 20°C !!!!
When temperature gets over a certain point (rough guess, about 40°C) a runaway reaction will occur, which itself generates
a lot of heat, and thus is self-sustaining. If, due to some crazy, totally "out there" reason, runaway does occur,
try to stay as calm as possible. Pour the entire red fuming and bubbling mix in at least the double volume of cold water.
The reaction will stop, and you can go extract your NG, no harm done (if you don't suffer a heart-attack)
BTW: If you do happen to suffer a hearth attack (wuss) you might want to use the stuff you just made,
Dip your finger in the NG and put it in your mounth, it will taste very sweet, and you'll get a head-ache
within a minute, that's because the nitroglycerine widens your blood vessels in your brain, but I guess it beats dying.
You don't want more then 0.25 ml in your body, because then you'll prolly go pretty sick ...
Now let's get busy
First mix the H2SO4 with your favourite nitrate salt (mine is NH4NO3). A little sidenote;
in this synth I use NH4NO3, because it makes the mix easier to stir, and far less crumbly (especially towards the end),
thus lowering the chance of hotspots in the reaction from occuring and giving a scary runaway reaction.
Here, the NH4NO3 and H2SO4 are mixed, and standing in an ice bath.
Now wait untill the temperature has dropped to around 10°C, and then slowly start adding glycerine.
Begin with the addition as a drop by drop process, and watch how the temperature evolves.
After each individual addition, you must stir the mix, so the glycerine can't form a layer above the acids.
If the temperature gets around 17°C, immediatly stop the addition, and keep stirring to distribute the heat evenly.
When it has cooled down again, you can resume adding the glycerine in small portions at a time,
constantly keeping one eye on the thermometer.
When all the glycerine is added, allow your mixture to cool to the absolute lowest temperature
your ice-bath can achieve. Because next step is to water the acid down, wich will produce
some heat too. Use cold water for this and you'll be fine, just pour it all in at once.
You'll notice some white blobs in the bottom of the reaction vessel. This is your NG !!
Now you'll need to get the pH of the solution up (less acidic). Easiest way of doing this is to decant, and add more water.
You better do this at least twice (depending on the size of your beaker). I first added
300 ml of water, decanted, added again 300 ml of water, decanted again.
(Sidenote due to many questions: Decanting is pouring the excess water acid mix off)
When done it could very well look like this ...
Now it's time to get the water out of your trinitroglycerine (that's why it's white)
I do this by adding to the NG , at least 200 ml of saturated NaCl solution (table-salt).
Make sure there are no more salt crystals left, otherwise, it'll sink in your nitroglycerine,
making it more likely to detonate from shock or friction. (NOT good !!)
So when the saturated table-salt solution is added, you'll just have to wait for it to clear out.
Giving it an occasional stir is good I think, opening up new surface area on the blob of NG.
I left mine overnight, so guess what, I'm off to bed now !!! (making this page took longer then synth !!! )
This is the blob on day 2 (left pic) and on day three (right pic) ...
In meanwhile, if you're bored or something, you could start to manually remove impurities.
just scoop them out with something, you'll figure something out ...
While waiting and having not much interesting to do, I cleaned up my lab :-)
So I waited, and waited, and finally, after 4 days it was clear !!!
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EDIT: F*uck the waiting with the sturated salt solution, just make sure it isn't acidic
by leaving it long enough under basic solution, and then suck the NG from under the water
(I used a syringe), and place it in a shallow dish in a dessicator (closed vessel with water absorbant).
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At this point, make sure that the NG is neutral, if need to, leave it for another day
under a basic solution, with some good stirring now and then.
Then I removed as much water as possible with a syringe, and left the NG in a shallow container
to let the rest of the water evaporate off. This also takes quite some time. Make sure it's
in a place where no dust can fall in it, and where it can stand relatively undisturbed.
The final product: 10 ml of pretty pure trinitroglycerine !!
So now my little vial is full again with nice clear NG ...
Seems like time for some more testing ;-D
The reaction when it detonates:
4C3H5(NO3)3 (l) --> 12CO2 (g) + 10H2O (g) + 6N2 (g) + O2 (g)
You notice for every 4 molecules of NG that detonate, you get 1 molecule of O2 left over ...
So you may add some fuel when planning to give the NG some action.
I guess any fuel will do, as long as it's not acidic.
For example Al powder, active C or graphite, ...
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EDIT:
It looks like I'm pursuing that fuel thing, as I just made a little under 25 ml nitroglycerine
(with the method from the other edit), for testing performance when fueled.
Try not to drool when you look at this, it makes my hand slippery ...
Yup, that is 20 ml (30 gram) neutral pure and yummie trinitroglycerine :)
About a stick of dynamite I think ...
This is the same NG with 1.5 gram homemade nitrocellulose (in acetone solution)
and 1.5 gram 400 mesh flake Aluminium powder added to it.
While the acetone is evaporating out of it, some ideas on power comparing that are easy to realise with limited funding ?? => brainfevert@yahoo.com
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