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wessonsmith
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Synthesis of ETN & Fuming Nitric Acid
I am trying to decide if I should go through the trouble of a synthesis video for ETN and Fuming Nitric acid. My ETN synthesis method is based on the
1928 patent method which does not require any cooling of the mixed acids.
My Fuming Nitric Acid synthesis produces 300mL in 1.15hrs from 850g Potassium Nitrate and 510mL 98% Sulfuric Acid.
So, with 180g of Erythritol and the 300mL of Fuming Nitric acid, and an additional 440mL of 98% Sulfuric Acid(dehydration of the Erythritol) I can
produce approx 285g - 300g of 2x recrystallized ETN.
Total cost breakdown for the main precursors:
ETN Manufacture (180g)
Erythritol 180.0g $1.92
98% Sulfuric Acid 440mL $6.98
94ish% Nitric Acid 300mL $10.54
I have done this synthesis many times so I have it down to a science. I even have a simple method to eliminate dangerous NO2 gases from escaping from
the Fuming Nitric acid synthesis. All of my equipment can be purchased from eBay.
I have seen other synthesis videos of both ETN and Fuming Nitric acid and they seem cumbersome and/or time-consuming for very little product.
If someone else has already done this with equally good results, please post a link. Thanks!!!
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underground
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Why do you bother with FNA for ETN synthesis. You can just use directly 200g H2SO4, 65g kno3, 15g E. Do you think the extra effort worth for a bit
better yields ?
You actually use 180gE, 850g
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wessonsmith
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Quote: Originally posted by underground  | Why do you bother with FNA for ETN synthesis. You can just use directly 200g H2SO4, 65g kno3, 15g E. Do you think the extra effort worth for a bit
better yields ?
You actually use 180gE, 850g |
For me, the synthesis of FNA is very fast and easy. Plus no NO2 fumes, which is a big plus. From what I have seen, the yield using my
method is much better using FNA than the method you described.
Yes, I use 180g of Erythritol and 850g KNO3. I do this amount because my FNA production uses a 1000mL round bottom flask limiting my FNA
to 300mL. So 300mL of FNA is enough to convert 180g of Erythritol into 300g of ETN.
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Rocinante
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There is a guy on BitChute that claims/shows ETN synthesis with 100 g of 96 % SA (some 60 ml), 40 g of ammonium nitrate and 10 g E with near 100 %
yields - i.e. about 23 g of ETN. He starts at - 18°C.
His synthesis would be the cheapest one, I tried it and got only 11 g of product. Not sure about his way because of it.
https://www.bitchute.com/video/XrjpCnYs7fVL/
[Edited on 3-7-2019 by Rocinante]
[Edited on 3-7-2019 by Rocinante]
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underground
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ETN yields are almost never that high just like some patents or guys say. Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed
acids yields go high. That is why nowdays i use PE instead of E.
[Edited on 3-7-2019 by underground]
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wessonsmith
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| Quote: Originally posted by Rocinante | There is a guy on BitChute that claims/shows ETN synthesis with 100 g of 96 % SA (some 60 ml), 40 g of ammonium nitrate and 10 g E with near 100 %
yields - i.e. about 23 g of ETN. He starts at - 18°C.
His synthesis would be the cheapest one, I tried it and got only 11 g of product. Not sure about his way because of it.
https://www.bitchute.com/video/XrjpCnYs7fVL/
[Edited on 3-7-2019 by Rocinante] |
Actually, according to my math, it's not cheaper.
His method:
Erythritol 180g
NH4NO3 720g
H2SO4 1800g (984mL)
V.s
My method:
Erythritol 180g
KNO3 850g
H2SO4 950mL(total SA for Nitric production and dehydration of Erythritol)
Plus his method takes a lot LONGER and makes a fuming mess plus the danger of a runaway. When you factor in your getting 11g of ETN
which sounds about right, his method is dangerous and time-consuming for resources used. Not to mention I am making 300g of ETN with a 2000mL
reaction vessel. His method would require a MUCH larger reaction vessel to get it to work and trying to keep the reaction mixture cool with that much
stuff would be impossible. In fact, by the looks of it, his method would be almost impossible to make more than 60g of ETN. The cooling would be
next to impossible.
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caterpillar
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There is no need in distillation if you wanna make ETN. Use AN, dissolved in H2SO4 instead. If you make conc NA, use it for RDX or HMX.
Women are more perilous sometimes, than any hi explosive.
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wessonsmith
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| Quote: Originally posted by underground | ETN yields are almost never that high just like some patents or guys say. Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed
acids yields go high. That is why nowdays i use PE instead of E.
[Edited on 3-7-2019 by underground] |
You are correct about yields. I like ETN over PETN because of the OB% I take advantage of this with my Thermobaric mixtures as well as my ETN/NHN
binary Composition. More bang from the synergy. Plus Erythritol is sold on Amazon with no chance of being put on a watch list when you by 20lbs
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wessonsmith
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| Quote: Originally posted by caterpillar | | There is no need in distillation if you wanna make ETN. Use AN, dissolved in H2SO4 instead. If you make conc NA, use it for RDX or HMX.
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Using the method you describe, how much ETN can you produce at a time?
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twelti
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Distilling seems like a hassle, and a certain element of risk IS involved. Takes up space and time, which I have the least of. FNA is more dangerous
to handle and store than 70% NA. I don't see how saving a few dollars on yield factors into the equation one way or the other, at least not for me,
and the amounts I'm interested in using. Could be useful in the future however, so keep posting!
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wessonsmith
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Thanks for the feedback.
[Edited on 3-7-2019 by wessonsmith]
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twelti
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| Quote: Originally posted by underground | Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed acids yields go high. That is why nowdays i use PE instead of E.
[Edited on 3-7-2019 by underground] |
Are you just using the standard procedure but going up to 70 rather than 50 degrees at the end?
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underground
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70+ at the end. Yea standard procedure just like ETN. ETN will decompose at such temps but PETN wont.
[Edited on 3-7-2019 by underground]
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wessonsmith
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| Quote: Originally posted by underground | 70+ at the end. Yea standard procedure just like ETN. ETN will decompose at such temps but PETN wont.
[Edited on 3-7-2019 by underground] |
Yeah, I nitrate my ETN at 55°C. Been doing that since day one, 3 yrs ago.
[Edited on 3-7-2019 by wessonsmith]
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underground
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I nitrate ETN at max 23°C. If i go above 30°C it will decompose (kno3/h2so4 method).
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wessonsmith
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Using your method, how much ETN can you produce per session.
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underground
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What do you mean by "per session". My yields are about 65%. You can scale it up as much as you want.
[Edited on 4-7-2019 by underground]
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wessonsmith
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| Quote: Originally posted by underground | What do you mean by "per session". My yields are about 65%. You can scale it up as much as you want.
[Edited on 4-7-2019 by underground] |
What I was trying to ask was how much you can make at one time. The reason why I ask is it seems with the method you are using it would be very
difficult to keep a larger amount cool.
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underground
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You can put the H2SO4 into deep freeze and procced with a lot of ice. Than is for ETN. For PETN is quite easier cause it is not that sensitive to
temperature like ETN.
[Edited on 4-7-2019 by underground]
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Rocinante
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65 % yields using KNO3? Can you give us the exact ratios/procedure?
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underground
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200g H2SO4, 65g kno3, 15g E. Fine powders and completely dry from a desiccator bag. H2SO4 boiled down to azeotrope (98%). Add KNO3 to H2SO4 by keeping
temp below 10C. After addition of KNO3 completed, drop the temp below 6C then add E i small portions while keeping temp below 6C. After the addition
of E completed, keep below 6C for 15min. Then slowly increase the temp to 22-23C max for about 30min. Always maintain vigorous stirring
[Edited on 4-7-2019 by underground]
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twelti
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Strange batch
I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited
until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before
using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a
salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does
not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens
up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat
in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I
immediately stirred back into the rest of it.
Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if
I should be concerned. I normally get fine crystals, like snowflakes.
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wessonsmith
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| Quote: Originally posted by twelti | I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited
until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before
using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a
salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does
not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens
up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat
in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I
immediately stirred back into the rest of it.
Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if
I should be concerned. I normally get fine crystals, like snowflakes. |
I have made ETN about 25+ times. I usually make 300g at a time. My mixed acid method is 180g Erythritol that I first dehydrate in 440mL of 98%
Sulfuric Acid. This requires some cooling with an ice bath. I can add the 180g of Erythritol to the Sulfuric Acid in about 20 min, 10min if I add AN
to the ice. You will need to keep the temperature below 40°C or your Erythritol will carbonize. Once all the Erythritol has been added I then add
that mixture to my Fuming Nitric acid in (4) separate additions. So approx 175mL at a time. I need to apply heat so I can get the mixed acid
Erythritol mixture to 55°C reaction temperature.
Try dehydrating your Erythritol in Sulfuric Acid first, then temperature control won't be such an issue.
[Edited on 6-7-2019 by wessonsmith]
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twelti
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| Quote: Originally posted by wessonsmith | | Quote: Originally posted by twelti | I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited
until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before
using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a
salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does
not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens
up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat
in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I
immediately stirred back into the rest of it.
Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if
I should be concerned. I normally get fine crystals, like snowflakes. |
I have made ETN about 25+ times. I usually make 300g at a time. My mixed acid method is 180g Erythritol that I first dehydrate in 440mL of 98%
Sulfuric Acid. This requires some cooling with an ice bath. I can add the 180g of Erythritol to the Sulfuric Acid in about 20 min, 10min if I add AN
to the ice. You will need to keep the temperature below 40°C or your Erythritol will carbonize. Once all the Erythritol has been added I then add
that mixture to my Fuming Nitric acid in (4) separate additions. So approx 175mL at a time. I need to apply heat so I can get the mixed acid
Erythritol mixture to 55°C reaction temperature.
Try dehydrating your Erythritol in Sulfuric Acid first, then temperature control won't be such an issue.
Remember, the more water you are adding the hotter the reaction is going to be. So using 70% Nitric Acid means you are adding a lot of water which
means a lot of heat generation.
[Edited on 6-7-2019 by wessonsmith] |
Thanks for your hints. Dang, that is a lot of ETN you have made!! I can see why yield is very important to you. I did try the other method,
dissolving in SA first, on the last batch. Yield seemed about the same, though I've not controlled all variables in order to make a good comparison.
I don't have FNA, and haven't felt the need yet, though I know there are some advantages.
Upon reX, I got a gram or two of material not dissolving in the EtOH. I filtered that out. It is very slightly yellow, and dull colored. The rest
came through with flying colors. Bright white and twinkly like mica, just like before. My stir rod might have got stuck. I've noticed if I turn it
up too fast, after the liquid gets thick, it just starts jumping around and not stirring. It is also harder to see in there as the nitration goes on.
I didn't go up anywhere near 55 degrees in the nitration. Im getting around 70% yield (AFTER reX).
I bought a microscope to look at the crystals. I'm having a hard time correlating my product to others description of crystal form. My ETN comes out
looking like snowflakes in suspension, and almost like a paste after final filtering. I'm doing reverse Rex in hot EtOH, using icecube "seeding" and
then pouring cold dH2O slowly into vigorously stirred EtOH.
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wessonsmith
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| Quote: |
I did try the other method, dissolving in SA first, on the last batch. Yield seemed about the same, though I've not controlled all variables in order
to make a good comparison. I don't have FNA, and haven't felt the need yet, though I know there are some advantages.
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Just an FYI, my yields are based on maximizing my Fuming Nitric Acid precursor and not the Erythritol. 180g of Erythritol converted to 300g of ETN is
a lousy yield when based on the theoretical maximum conversion of Erythritol to ETN. However, since the precursor Erythritol is now 10x less
expensive to use than Fuming Nitric acid, I tweaked the ratios to maximize the Fuming Nitric Acid precursor.
The reason for dehydrating the Erythritol in Sulfuric Acid first is 1) Safety; no chance of a runaway once the Erythritol has dehydrated. 2) Ease of
manufacture; temperature control is much easier when you are heating rather than cooling. This advice only applies to Fuming Nitric Acid. When you
are using 70% Nitric Acid, you are introducing water which when mixed with the acids generates heat.
You need higher temperatures so that you can easily mix your nitration mixture with a stir bar. At the higher temperature, the ETN remains dissolved
in the acids. When the mixture is allowed to cool below 45°C, ETN starts to crash out, causing the mixture to thicken up considerably, making
stirring with a stir bar next to impossible. Allowing the nitration mixture to thicken up before all of the Erythritol has converted, you increase
the possibility of localized excessive heat, which destroys some of the ETN.
Once you start using Fuming Nitric Acid, all of the issues you are having will go away. I can't stress enough just how easy and relatively
inexpensive it is to manufacture Fuming Nitric Acid.
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