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twelti
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[*] posted on 7-4-2019 at 14:12


Quote: Originally posted by snooby  
Why are you sure you have failed? Most nitro esters just burns, but only detonate from inpact. Thats why its called secundary explosive. So in case if you havent tried it, go do some hammerblowntests. Maybe the etn is just fine.


Hi, yes I did try that. Melted it a little, then whack. I did manage to get maybe 1 out of 5 to go that way. I did see on YT where he was just laying some on a piece of foil and with flame , getting high order dets. Mine just defllag so far. I wonder if it is not fully dry? Gonna try another synth, this time letting temp go up to 25 for é0 min. And dry in dessicator.

UPDATE: repeated it but this time added 30 min letting the mixture slowly to up to 27 C and stay. Yield looks to have doubled, at least the before reX yield. 5.5 g E gave 15.5 g moist (pressed) neutralized product. Guessing alot of that is water, but still... Now for the reX.

[Edited on 8-4-2019 by twelti]
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Laboratory of Liptakov
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[*] posted on 8-4-2019 at 21:10


We are curious on your pure yield with " 27 C and stay".....:cool:...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....:cool:....LL

[Edited on 9-4-2019 by Laboratory of Liptakov]




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[*] posted on 9-4-2019 at 03:47


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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[*] posted on 9-4-2019 at 11:53
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?!


20190407_111738.jpg - 4.4MB 20190407_183045.jpg - 3.4MB
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[*] posted on 9-4-2019 at 12:23


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,
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[*] posted on 9-4-2019 at 14:56


Are you 100% that what you use for nitration is pure erythritol ?
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[*] posted on 9-4-2019 at 15:28


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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[*] posted on 9-4-2019 at 19:16


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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[*] posted on 10-4-2019 at 01:06


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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[*] posted on 10-4-2019 at 03:39


Quote: Originally posted by C6(NO2)5CH2CH(CH3)N(NO2)2  

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)


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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[*] posted on 12-4-2019 at 12:32


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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[*] posted on 13-4-2019 at 07:13


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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[*] posted on 13-4-2019 at 11:18


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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[*] posted on 13-4-2019 at 11:39


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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[*] posted on 13-4-2019 at 12:09


OK.....:cool:....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....:cool:...LL



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[*] posted on 16-4-2019 at 04:47


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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[*] posted on 16-4-2019 at 12:24


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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[*] posted on 16-4-2019 at 23:42


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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[*] posted on 18-4-2019 at 13:25


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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[*] posted on 15-5-2019 at 13:41


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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[*] posted on 15-5-2019 at 20:47


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 ?


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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[*] posted on 16-5-2019 at 11:52


So ANFO more sensivite than UN. Interesting.
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[*] posted on 23-5-2019 at 07:39


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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[*] posted on 23-5-2019 at 11:20


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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[*] posted on 23-5-2019 at 11:40


You can use caramelit...... https://www.youtube.com/watch?v=nMfCzjMLz3w ......:cool:...LL



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