|  Author | Topic: Erythritol Trinitrate (Read 298 times) |
kataklysm
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Karma: 2 |  | Erythritol Trinitrate
« Thread Started on Nov 10, 2007, 2:53am » | ![[Quote]](http://s4.images.proboards.com/buttons/quote.gif) |
ETN
Step one
Chill 17mL of sulfuric acid on an ice bath to 0° C then slowly add 30g KNO3, it wont fully dissolve. The mix will become thick and produce white nitric acid fumes.
Stir in 7.5g of erythritol keeping the temperature below 15° C.
Step two
While stirring the acidified erythritol mix slowly pour in the remaining 33 mililiters of H2SO4 at a rate of about 1mL every few seconds. The mix will become easier to stir as more sulfuric acid is added.
What's happening in this reaction?
Sulfuric acid is stripping away hydroxyl groups from the erythritol and the protonated hydrogen from nitric acid and absorbing the water that is produced. Concentrated sulfuric acid is acting as the limiting reagent, once it has absorbed enough water it will no longer attack the polyol. This means less chance of destroying unnitrated or partially nitrated erythritol.
HO- + H+NO3- → NO3- + H2O
The ETN is left to nitrate for 15 minutes after the last addition of H2SO4, stirring occasionally.
Filtration, washing and purification
Crash the acidic ETN into 0.5 liters of cold water and stir it around until all the solubles have dissolved. A fine white precipitate of ETN will appear.
ETN precipitate
Snow-like precipitate of ETN.
Filter and thoroughly wash the ETN before neutralizing and washing again.
To purify simply dissolve the ETN crystals in excess acetone, heat until boiling then crash into cold water and filter.
Safety
Store dry away from heat and light.
ETN slowly decomposes if stored in a warm or acidic environment.
Uses
Detonation occurs as 2 C4H6N4O12(s) → 6 H2O(g) + 8 CO2(g) + 4 N2(g) + O2(g) OB: +5.30
ETN can be substituted for PETN in many applications, like detonating cord. It is soluble in nitroglycerine which makes a very oxygen rich plasticizer.
Making use of its very low melting point, ETN can be melted and cast into casings by heating with steam or hot water.
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rauhuljadid
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« Reply #1 on Nov 10, 2007, 6:42am » | |
hi there, nice forum....
how about nitrating glucose, for my theory, it would be glucose hexanitrate right?
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kataklysm
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« Reply #2 on Nov 10, 2007, 12:51pm » | |
hmm... I do belive so but I am not 100% sure I will do a bit of research and get back to you.
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enkidu
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« Reply #3 on Nov 10, 2007, 8:41pm » | |
Quote:What's happening in this reaction?
Sulfuric acid is stripping away hydroxyl groups from the erythritol and the protonated hydrogen from nitric acid and absorbing the water that is produced. Concentrated sulfuric acid is acting as the limiting reagent, once it has absorbed enough water it will no longer attack the polyol. This means less chance of destroying unnitrated or partially nitrated erythritol.
HO- + H+NO3- → NO3- + H2O |
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Your mechanism is a bit messed up...
nitric acid + sulfuric acid ---> nitronium ion + bisulfate ion + water
nitronium ion + hydroxyl group + bisulfate ion ---> nitrate group + sulfuric acid
Sorry, I'm to lazy to do all the tags (I've done had to do them in several other posts on this exact topic).
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trashcanman
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Karma: 0 | | Re: Erythritol Trinitrate
« Reply #4 on Nov 12, 2007, 4:50pm » | |
Quote:hi there, nice forum....
how about nitrating glucose, for my theory, it would be glucose hexanitrate right? |
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According to my research Glucose can be nitrated, but I wont be doing it any time soon.
It takes extreme measures,(99% HNO3) and it is way more dangerous than NG.
You must keep it sub-zero, or you will have a runnaway.
Oh and the max is penta-nitrate.
It is supposed to bey very powerful, but not very practical.
PS. I am doing a course in organic chemistry ATM so I wont be very active here, or anywhere else for a little while.
But, I'll be back 
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rauhuljadid
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Karma: 0 | | Re: Erythritol Trinitrate
« Reply #5 on Nov 14, 2007, 11:51pm » | |
you wont doing that huh? so, whats the reason, why did u saying that the reaction must be in sub-zero condition?
Did the reaction produces a lot of energy and very unstable?
how about the............ Hexanitrohexaazaisowurtzitane and Octanitrocubane???
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johnhinckley
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« Reply #6 on Nov 15, 2007, 11:03pm » | |
This is a good method, although I like to scale it up.
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trashcanman
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Karma: 0 | | Re: Erythritol Trinitrate
« Reply #7 on Dec 1, 2007, 6:38am » | |
Hey kataklysm, have you detonated your ETN yet. I detonated mine today, VERY NICE.
Did you purify/recrystalize it. I didn't, as I use lab grade H2SO4 & HNO3, I don't believe purification is necessary.
I am going to be doing some mega det's in the next month or so, i'm in the process of getting Al powder to perfect the oxygen balance of my NG and bring it to it's full potential.
When I finish my chemistry course,(in the next couple of months), I will also post my synths.
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trashcanman
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Karma: 0 | | Re: Erythritol Trinitrate
« Reply #8 on Dec 1, 2007, 9:09pm » | |
Quote:
how about the............ Hexanitrohexaazaisowurtzitane and Octanitrocubane??? |
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What the hell have those compounds got to do with nitrating glucose.
The first one is a nitro-amine, and the second, a nitro compound,
Either way both are completely irrelevant to nitrating glucose.
Glucose can be nitrated, but it is a nitric ester, the nitro groups attach to the hydroxyl groups, of which glucose has 5, so as I said penta-nitrate is the max.
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trashcanman
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Karma: 0 | | Re: Erythritol Trinitrate
« Reply #9 on Dec 16, 2007, 5:34am » | |
I just noticed, (apparently no-one else has either), that the title of this thread say's erythritol trinitrate, where it should say tetranitrate.
Anyway that being said here is my method of synthing ETN.
Step 1
Prepare a nitration bath of 2 parts 98% H2SO4 to 1 part 70% HNO3. For this synth I used 150ml H2SO4 -- 75ml HNO3.
measure out the H2SO4 place it in the reaction vessle, then place the vessle in a salt ice bath. Achieve the lowest temp your bath will get to, then slowly add the HNO3 so as to not let your temp jump,(I never let it get above 10 degrees celcius).
When all the HNO3 is added allow your ice bath to cool it down below, or as close to zero as you can.
Step 2
When your nitration mix is as close to or at zero, begin the addition of the erythritol. For this synth 25 grams.
Add it about 1 gram or a little less at a time, constantly keeping an eye on the temp,I keep it between 0 and 5 the whole time, as well, keep a slow even stirring the whole time.
It took me just under an hour to add all 25 grams.
After adding the last of the erythritol I have a milky mixture around the consistency of thin cream.
I allowed 17 mins of nitration time from the moment of the last addition of erythritol.
Step 3
Now after allowing the mix to nitrate for 17 minutes, it was crashed into 2 litres of chilled distilled water.
The ETN precipitated out like snow flakes.
Step 4
Now it's time to filter and clean up.
I use coffee filter's. Once all the crystals are collected, I give them a thorough wash with distiled water, then a thorough wash with NaHCO3, then a final thorough wash with distilled water.
I don't bother to re-crystallize, as I believe with pure reactants this is not essential, and I have not yet come across a problem with stability,(very stable), or power.
Using this method I recovered 22 and a bit grams of ETN from 25 grams of erythritol, and I lost a fair bit during filtering and cleaning, I believe my yield was very close to 100%.
Now it's just a matter of drying your crystals and away you go.
Here is the vid of the 22 grams of ETN from the above synth being detonated
http://www.youtube.com/watch?v=qt6hJ3stquM
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