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VladimirLem
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wtf?
u're getting stroppy cause the steel-target havent got more damage?
how about putting the ignitor ONTOP of the charge (like a shaped charge) to force the detonation to move towards the steelplate and not to the side of
the charge? 
[Edited on 15-3-2013 by VladimirLem] |
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SherlockHolmes
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Exactly detonator had to do but I knew until after the test 
Sorry for my english. I am not from England. Thank you!
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Ral123
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I had s cup of water/ammonia with MN on the bottom for storage. It appears the MN dissolves in the water and evaporates from the top, even trough the
layer is on the bottom. After a week there's no MN in the cup, only water. Is it possible that some other process has taken place?
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WGTR
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This looks like the generic methyl/ethyl nitrate thread, so I think this is the right place to post this.
I have an issue that might seem unusual. I'm trying to not make ethyl nitrate. I'm actually interested in making glyoxal
(to synthesize ionic liquids), and am trying to avoid performing any unintentional nitrations. This is basically a sanity check of sorts, to make
sure that I'm not doing something stupid. I have little experience reacting nitric acid with organics, so I'm approaching this with caution.
Debus originally made glyoxal by oxidizing ethyl alcohol slowly with nitric acid at "ordinary temperatures".
Philosophical Transactions of the Royal Society of London, Volume 148
Generally they would do this by carefully pouring the alcohol on top of the acid, so that two layers would form without mixing. The reaction would
gradually occur by diffusion of the two layers.
My old friend Debus was a very smart guy, but he lived during a time when people pipetted chemicals with their mouths, and tasted unknown substances
to identify them. I hope he will forgive me for not trusting his procedures 100%.
A newer patent is a bit more descriptive, but starts directly from acetaldehyde:
Attachment: US3429929.pdf (224kB)
This file has been downloaded 702 times
I intend to use the methods from the patent, but rather start from ethyl alcohol instead, to attempt performing a one-pot reaction.
Basically, the plan is to react 0.5% copper(II) oxide (catalyst) with 50% nitric acid solution. A small amount of sodium nitrite (initiates
reaction) will be added to absolute alcohol, and then the nitric acid will be slowly added under stirring to the alcohol (maybe over 1-2 hours). The
temperature will be maintained at 40°C with a water/ice bath. Naturally, this will have to be done on reflux to keep the acetaldehyde from
escaping.
Note that I'm forming nitrous acid in situ, that there is water in the reaction (50% nitric acid), and that the acid is being added slowly to keep the
temperature at 40°C.
Am I properly avoiding the conditions that would perform a nitration?
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ManyInterests
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Since I want to make some methyl nitrate to experiment with mixing it with nitrostarch to see if it does form a kind of plastic explosive with that, I
just do have some questions to ask mostly about some safe storage and disposal since it could be a few weeks before I use it. Someone mentioned that
putting it in a fridge or even freezer in a sealed container can be a good way of preserving it. Is this correct?
As for how I intend to make it. I will be making it in a simple nitration mixture. The proportions will be taken from the improvised munitions
handbook (80ml of methanol, 145ml of 95% sulfuric acid, and 95ml of azeotropic nitric acid) and I will be washing it with a saline solution and drying
with calcium chloride.
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Microtek
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I agree that well neutralized, washed and dried methyl nitrate could probably be stored for a long time in a sealed container made of a suitable
material. Putting it in the freezer could also be a good idea since one of the big issues with methyl nitrate is its volatility.
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ManyInterests
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This webpage documents the cleaning process I will follow, but not the synthesis. It involves a lot of washing, which is something I am
comfortable with. Especially with ice cold water since methyl nitrate is not very soluble in very cold water and it loves being cold.
For the synthesis, I will cool down the nirating mixture on its own in the freezer for at least 12 hours and I will also have a large glass bowl of
ice water to float it in while I add the mixture. That way if anything seems wrong I can immediately overturn the beaker into th water and prevent an
accident.
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dettoo456
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If you’re planning to store the MeONO2 too, aside from it being in a freezer, make sure to vent it at least 1X a week and make sure to limit its
exposure to UV as much as possible.
Try to invest in a full face shield (or full face respirator) and a Kevlar scarf too; glass shrapnel is no joke 
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ManyInterests
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Quote: Originally posted by dettoo456  | If you’re planning to store the MeONO2 too, aside from it being in a freezer, make sure to vent it at least 1X a week and make sure to limit its
exposure to UV as much as possible.
Try to invest in a full face shield (or full face respirator) and a Kevlar scarf too; glass shrapnel is no joke |
I have both. I have kelvar sleeves I can use to make a scarf.
I won't store it for long. Like maybe I will keep it for 10 days or so at the most. I might not put it in a glass container, but rather a plastic one
I might wrap it plastic wrap.
If you look at the proportions I will be using, the end product might be over 100 grams Not sure if anything can protect me if it goes off... just how
sensitive IS methyl nitrate? I saw videos where people smacked it really hard with heavy hammers (on makeshift steel anvils, too) and it did not
detonate.
When I make it into a charge, I'll be using a cardboard tube with an epoxy plug on one end, I am thinking of closing the other end after I insert the
detonator (a 1g melt-cast ETN charge with 0.3g of ETN:NHN mixture in a .223 Remington case... an overkill I know) This will make venting impossible,
and when the epoxy hardens, it generates a lot of heat. I will be doing this the night before I go to see how much of a bang it makes.
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Sir_Gawain
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Why don't you make it into dynamite? It seems like it would be much easier and safer to handle that way. Add methyl nitrate to a mixture of ammonium
nitrate and flour or fine sawdust until it is saturated, but not dripping.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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| Quote: Originally posted by Sir_Gawain | | Why don't you make it into dynamite? It seems like it would be much easier and safer to handle that way. Add methyl nitrate to a mixture of ammonium
nitrate and flour or fine sawdust until it is saturated, but not dripping. |
That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is
10:1 of methyl nitrate to nitrostarch.
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Sir_Gawain
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| Quote: Originally posted by ManyInterests |
That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is
10:1 of methyl nitrate to nitrostarch. |
Like blasting gelatin, great! A gel or plastic is much better than
liquid.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Microtek
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We've talked about excessively cold nitrations before. A mixed acid that is too cold can lead to runaway more easily than one that is the proper
temperature. I suggest you make a salt-ice bath and use that to cool the nitration mix to about 0 C, and then maintain the temp at 0-5 C by adjusting
the speed of addition of the methanol. That way, the reaction has a chance to approach equilibrium before too much substrate (methanol) is in the mix.
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ManyInterests
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| Quote: Originally posted by Microtek | | We've talked about excessively cold nitrations before. A mixed acid that is too cold can lead to runaway more easily than one that is the proper
temperature. I suggest you make a salt-ice bath and use that to cool the nitration mix to about 0 C, and then maintain the temp at 0-5 C by adjusting
the speed of addition of the methanol. That way, the reaction has a chance to approach equilibrium before too much substrate (methanol) is in the mix.
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Understood. I will cool the nitration mix in the fridge and not the freezer. That way it'll be closer to 0 C than -10C or so before the stuff is
added. I will also add the methanol slower than what the improvised munitions handbook recommends (half teaspoon (2.5ml) per minute or so. I will add
a little less than that amount every 3 or 4 minutes and monitor carefully.
I assume the same thing should be done with things like EGDN, DEGDN, and Nitroglycerine?
| Quote: Originally posted by Sir_Gawain | | Quote: Originally posted by ManyInterests |
That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is
10:1 of methyl nitrate to nitrostarch. |
Like blasting gelatin, great! A gel or plastic is much better than
liquid. |
Yep, I wonder why anyone thought I would be using plain methyl nitrate. I got the idea from Tim Lewis's kitchen improvised explosives. I did ask
around and it seemed that the idea of nitrostarch mixing with a liquid explosive to form a putty is quite plausible, and it will be more stable than
plain methyl nitrate. Albeit it must still be used ASAP.
Even the Improvised Munitions Handbook section on methyl nitrate has instructions to use it as a dynamite. They suggest using shredded cloth, paper,
or sawdust as an absorbent material. I did not know that flour could work, too. I am also guessing that diatomaceous earth would work well with methyl
nitrate.
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ManyInterests
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OK, so I am going to give my after synthesis report. Currently it is not 100% finished as I drying it with calcium chloride in the freezer as per the
cleaning instructions. I made one mistake: I forgot to give it a 2nd salt-water wash after the sodium hydroxide deacification, I used simple ice-cold
water, the water is very slightly acidic, but I am not sure if it is from the methyl nitrate... I didn't want to lose too much through washing. It is
very, very slightly acidic so it probably doesn't matter. Or maybe I am wrong. I lost around 10g from the whole thing. But all in all I am quite happy
with the yield. Also there is no discoloration whatsoever in my yield, which is also very pleasing to know.
The nitration itself was highly uneventful and completely boring. Neutralizing the leftover acid was SCARY, when I added simple water to it, it turned
green and emitted a lot of NO2. I did not inhale any, thankfully, and neutralizing it with water and bicarbonate also had a lot of gasses come out,
which I combated with my mighty spray bottle of bicarbonate solution.
The calcium chloride has thickened up quickly, I assume it has absorbed the water. I will need to treat it a 2nd time with calcium chloride according
to the instructions to fully dry it. I used around 5 or 6 grams, I will use another 5 or 6 grams.
I will use my nitrostarch to make it into a plastic explosive immediately before putting it in the freezer.
[Edited on 28-7-2024 by ManyInterests]
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ManyInterests
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OK, so the guide giving the proportions of 1 gram nitrostarch to 10 grams of methyl nitrate was a lie. I needed a LOT more nitrostarch to get it to
gel up, and it was not a play-dough like consistency but more like a very thick regular dough. I might have gotten a whiff of the nitrate as I was
mixing since I felt mildly light headed, I did the process in the most well ventilated area in my apartment. I stopped counting how much nitrostarch I
put in. but I am very glad I had enough for it. (and if I didn't, i guess regular cornstarch and flour would suffice?).
After mixing the stuff was so thick that I left the spoon in and I wrapped the tupperware in many layers of plastic film. I will keep it there until
it is time to load it in its container. Then I will keep it in the freezer again until it is time to seal the other end with epoxy.
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Microtek
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When gelling a liquid nitrate ester such as methyl nitrate with nitrostarch or nitrocellulose, the colloidonization take time, especially at lower
temperatures. Did you wait for it to gel before adding more? Also, what temp was this done at?
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ManyInterests
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Now I feel extremely dumb. Yes it was ice cold. I had just finished drying it with calcium chloride (I treated.it twice with the stuff) and once I was
confident it was dry I started adding the nitrostarch. I hadn't done anything like this before and I wasn't sure what to expect.
It had been in the fridge and freezer while drying since the instructions were to keep it at 0C. I didn't wait too much between additions, so I must
admit I added a lot...
I guess next time I should wait more. At any rate it is done and I am keeping it in the freezer until it is time to take it out for use in around 12
to 14 days.
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