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Laboratory of Liptakov
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We are curious on your pure yield with " 27 C and stay"..... ...LL
next: My question for an Great scientist of this forum.: I do not find concentration for HClO4 according his boiling point. Especially for 140
Celsius.
Thanks for anyone........LL
[Edited on 9-4-2019 by Laboratory of Liptakov]
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underground
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Anhydrous perchloric acid is an unstable oily liquid at room temperature. Perchloric acid forms an azeotrope with water at 203°C, consisting of about
72.5% perchloric acid
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twelti
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ETN strangeness
OK, I'm a bit stuck here. I realize there is a TON of stuff on these forums about ETN synth, but actually 90% seems to be about nitrate salt
method(s). I really like the HNO3 idea since i have a bunch and it stirs easily.
Using a longer and warmer nitration period of 30 minutes at around 27 degree C, I did get a bigger yield from my first attempt. Everything looks like
it should have been a success, final yield of around 8 g from 5.5 g of erythritol. Also, this time I added ice cubes during the reX to "seed" the
crystalization. Material looks pretty much like the first time tough. Pressed between paper towels after final filtration, it is more of a cake. i
was hoping for better crystals, using the "add water to EToH" method, but it is same as before.
Small piece on foil heated: deflag and no residue.
Small piece melted and then wrapped in foil and whacked: after several attempts, it did sort of detonate,(i.e. sparks) but not very loud. Strangely,
if I whacked it again I often got a second spark. It did not all go off?
It has been drying for a day and a half now. Is it not dry? Should I give up and go nitrate salt method? I have some KNO3.... It is driving me
nuts though. What else can it be but ETN?!
 
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johnmay
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Hello twelti,
Maybe you should check it the other way - wrap it in alluminium foil and put it in the candle flame (not in your hand of course!), it should detonate
if it is okay.
ETN is not primmary material so I wouldnt expect it to go off from smacking it on the floor (I saw a yt video of some guys pounding it with big hammer
and for no go.
Take care,
Regards
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underground
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Are you 100% that what you use for nitration is pure erythritol ?
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C6(NO2)5CH2CH(CH3)N(NO2)2
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If it detonated even once, then I think you've got some ETN! The yield may not be as good as it could be, but you succeeded, I think. The rest would
probably go if it was dry and was triggered by a primary.
Now my own (probably dumb) question. Has anyone recovered H2SO4 from a nitration? Or is that just an altogether bad idea (eg. traces of explosive
product)
Put that in your pipe and smoke it!
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twelti
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Oh, Joy of Joys! As we speak, little fine bits of foil confetti are lazily floating down to the floor in my workspace! Not sure if if was the extra
drying, or the more aggressive confinement suggested, but I got nice high order dets now. Still not sure how that one guy on YT (https://youtu.be/ETs1pkz1Umk) got his to det, open on a piece of foil, but I guess the fact that it deos not go off ease with a hammer, or from
simple heating of small amounts is a GOOD thing. I also made a small straw with around 60 mg of ETN and 15 mg of SADS and that went off nicely too.
I guess it worked. Yield has a little room for improvement I guess. In my reX I also added some urea, I hope that works well. So far testing
neutral with a moist litmus. Will retest every week or so.
Speaking of that, it makes more sense to me to add the urea or whatever stab you are using in the solvent (EToH in my case). That way it has time to
work. I've seen others adding it in the crash solution. But in that case it wouldn't have vary long to act before new crystals are formed, seems to
me...?
[Edited on 10-4-2019 by twelti]
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underground
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Quote: Originally posted by C6(NO2)5CH2CH(CH3)N(NO2)2  | If it detonated even once, then I think you've got some ETN! The yield may not be as good as it could be, but you succeeded, I think. The rest would
probably go if it was dry and was triggered by a primary.
Now my own (probably dumb) question. Has anyone recovered H2SO4 from a nitration? Or is that just an altogether bad idea (eg. traces of explosive
product) |
I was thinking about the same and i have made a topic about this subject. My idea was to use AN/H2SO4 for nitration. After crashed and filtered, the
water will contain h2so4/ammon. sulphate maybe AN and unnitrated / partly-nitrated esters. During concentration of crude h2so4 all ammonia salts would
evaporate and the remaining unreacted esters would become carbon. In theory you will end with concentrated h2so4 with a little bit of carbon. I dont
thik so carbon would have any effect in final yields
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Herr Haber
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Depending what you plan to do with that H2SO4 it might be a bad idea.
Spent acid from TNT manufacture can be fortified again and used for the mono nitration.
Spent acid from nitroglycerine is mostly useless.
Urbanski should give you a few good ideas of what is doable but in most lab setups it's not practical to recover the spent acid.
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Laboratory of Liptakov
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For example was tested using nitration mixture firstly for nitrocellulose (14%N) and follow for ETN with yield 50%. Because NC is possible get out as
one piece of material of out.
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FeedMe94
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I was looking for a synthesis for nitration of erythritol and im a bit confused. The one synthesis i found was : 185ml of 68% Nitric Acid + 270ml
Sulfuric Acid 96 + 75g erythritol and the other was 395 grams ( not ml ) NA 68% + 756 grams of SA 96%
+ 75 grams of erythritol. Any help about how should i proceed ?
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Laboratory of Liptakov
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60 ml H2SO4 (96%) 40 ml HNO3 (65 - 68%) + 10g E. = 300 ml Nitric Acid + 450 ml Sulfuric Acid + 75g E. 1 ml SA = 1,85g
1 ml NA = 1,4g. On 10g E we need 111g SA + 56g NA. From this can be output 21 - 22g pure recrystallized ETN.
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FeedMe94
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| Quote: Originally posted by Laboratory of Liptakov | 60 ml H2SO4 (96%) 40 ml HNO3 (65 - 68%) + 10g E. = 300 ml Nitric Acid + 450 ml Sulfuric Acid + 75g E. 1 ml SA = 1,85g
1 ml NA = 1,4g. On 10g E we need 111g SA + 56g NA. From this can be output 21 - 22g pure recrystallized ETN. |
Thank you very much Dr. My head was a mess before that
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Laboratory of Liptakov
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OK.........PE is possible dissolve in NA only, and drop this transparent
solution into SA. Advantage 1: Nothing crushing PE before adding into NA+SA mixture. Advantage 2: Comfort adding, maximal yield. For E is this process
impossible. Arises zero yield.......LL
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FeedMe94
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I recrystalized my ETN using acetone. When i poured it into ice water the ETN participated as big chunks and not flour consistency as before. Does it
look ok ?
https://ibb.co/dB0mYDS
By the way whats ETN solubility in acetone cause i may use too much
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Laboratory of Liptakov
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Best results are usually from methanol, because has ideal solubility effect and because is usually pure. Ethanol contents impurities against
consumation and acetone also contents impuritires, usually some as the fat. Pure ETN should by look as mica platelets.
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FeedMe94
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| Quote: Originally posted by Laboratory of Liptakov | | Best results are usually from methanol, because has ideal solubility effect and because is usually pure. Ethanol contents impurities against
consumation and acetone also contents impuritires, usually some as the fat. Pure ETN should by look as mica platelets. |
I used acetone because its 99.9%. I cannot obtain methanol and the ethanol i have is 95%
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FeedMe94
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Tomorrow I'm going to try some Red Phosphorus with KCLO4 , KCLO3 , KMnO4 and NH4NO3 mixtures. Ofcourse not more than 100mg each. Could you give me
some ratios please? I know for KCLO4 and KCLO3 is 70/30.
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underground
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Which one is more sensitive urea nitrate or ANFO ? If UN is more sensitive, with what energetic its sensitivity can be compared ?
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FeedMe94
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| Quote: Originally posted by underground | | Which one is more sensitive urea nitrate or ANFO ? If UN is more sensitive, with what energetic its sensitivity can be compared ?
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Urea Nitrate
Melting Point: 152 ° C
Detonation velocity 3400 m/s at density
0.85 g/cm3
Lead block test 270 cm3
Impact Sensitivity: no reaction to 50 Nm
Friction Sensitivity: no reaction up to 353N
Nitrourea
(prepared by dehydration of urea nitrate with concentrated sulfuric acid)
Detonation velocity: up to 7000 m / s
Melting point: 159 ° C, decomposition
Lead block: 310 cm 3
Mildly sensitive to heat and shock
ANFO
Bulk density: 0.8 gr./cm3
Relative weight strength: 75%
Velocity of detonation: 3,000 m/sec
Strength (Trauzl Lead block test): 335 ml
Brisance (Hess test): 5,3 mm
Energy of explosion: 920 Kcal/Kg
Gas volume: 970 It/Kg
Explosion temperature: 2600oC
Friction sensitivity: >360N
Impact sensitivity: >50J
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underground
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So ANFO more sensivite than UN. Interesting.
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Metallus
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I'm interested in the chemistry (theory) behind the synthesis of RDX from methenamine + HNO3 and the reasons behind all the temperature adjustments
during its synthesis or how impurities affect the synthesis (eg NOx concentration, presence of sulfates or other salts, etc).
It's likely that there is already a thread with all this information, but looking for it proved to be difficult, considering the huge mole of forum
posts on this subject. Most posts are about the procedure or recipes, without an in-depth explanation of the reasoning behind all those parameters.
1) Patent US2859215A on RDX synthesis gives a temperature range between -10 and +40°C. Some other recipes found in the web employ an ice-salt bath
(-30°C). What changes with the temperature? The reaction is exothermic, so with lower T the theoretical yield increases at the expense of kinetics.
In this sense, I assume the suggested 20-30°C operational temperature is a compromise between thermodynamics and kinetics. Is that correct?
2) The addition of methenamine to WFNA has to be carried slowly. Is it because the reaction is dangerously exothermic and so it's necessary to let the
mixture cool down a bit between each addition in order to easily maintain the temperature < 30°C?
3) After the two reactants are mixed, the temperature is quickly raised to 80°C. Is it to speed up the reaction? Why the temperature must be raised
so quickly? What happens if it's raised gradually? Also why all that care to maintain it below 30°C in the first step if then you have to quickly
raise the temperature?
4) In order to precipitate the RDX crystals, the acid mixture is washed with cold water. Is it to counter the exothermic reaction between the leftover
HNO3 and water? Or is it to more easily allow the precipitation of the crystals? Or both?
5) How do impurities affect the reaction? Especially NOx dissolved in HNO3 or the presence of sulfates or other salts.
6) What is the most critical and dangerous step of this synthesis and why?
Thanks
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Simoski
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Are any copper salts fat soluble?
May not seem like an energetic material type of question, but if there are any I will disolve it is lard or tallow, add potassium chlorate and have me
a new blue / green pyrotechnic star mix
[Edited on 23-5-2019 by Simoski]
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Laboratory of Liptakov
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You can use caramelit...... https://www.youtube.com/watch?v=nMfCzjMLz3w .........LL
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Simoski
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I will, thanks LL, will make great flare mix!
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