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caterpillar
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??? Why? Salts are generally much more available. There are few compounds, that really require pure HNO3- RDX, HMX, nitroform (add something if you
wish). But generally the idea is clear- salts are more powerful nitrating agents for the very simple reason- they do not contain water. BTW, RDX can
be prepared with the aid of the usual mixed acid. And mixed acid can be easily prepared if you have Ca(NO3)2.
Women are more perilous sometimes, than any hi explosive.
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Herr Haber
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Quote: Originally posted by caterpillar  |
??? I love HE and I haven't written books. I described my own experience. I can only add, that KNO3 can be replaced with NaNO3, but do not use NH4NO3!
You'll get lots of NOx. If you dislike semi-industrial methods, divide all numbers by 20, 50 or even 100. And I used not a lab vessel, mate- no- I
used 3 liters glass jar with wide throat from-under cucumbers. And who told you that you need 16 liters of water just in one piece? Take three liters
of cold water (crushed ice is useful, but not necessary) and put into it 300- 400 ml of the reaction mix. Filter the precipitate and repeat this
process again and again. |
Are you Jared in disguise ? 
I dislike him and his "cool cookbooks".
One page he describes a normal lab synth, the next one looks like pilot plant production...
What's the point of putting that in a book except to prove you dont actually have a lot of hands on experience ?
If you actually DO a synth, why not post YOUR data ?
Jared just copies and pastes.
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hissingnoise
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| Quote: Originally posted by caterpillar | | BTW, RDX can be prepared with the aid of the usual mixed acid. And mixed acid can be easily prepared if you have Ca(NO3)2. |
(Ahem!) Mixed acid cannot be used for RDX as H2SO4 decomposes hexamine ─ and why would you use calcium nitrate for
HNO3 when the sodium salt is less hygroscopic and so much more convenient?
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caterpillar
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| Quote: Originally posted by Herr Haber | | Quote: Originally posted by caterpillar |
??? I love HE and I haven't written books. I described my own experience. I can only add, that KNO3 can be replaced with NaNO3, but do not use NH4NO3!
You'll get lots of NOx. If you dislike semi-industrial methods, divide all numbers by 20, 50 or even 100. And I used not a lab vessel, mate- no- I
used 3 liters glass jar with wide throat from-under cucumbers. And who told you that you need 16 liters of water just in one piece? Take three liters
of cold water (crushed ice is useful, but not necessary) and put into it 300- 400 ml of the reaction mix. Filter the precipitate and repeat this
process again and again. |
Are you Jared in disguise ?
I dislike him and his "cool cookbooks".
One page he describes a normal lab synth, the next one looks like pilot plant production...
What's the point of putting that in a book except to prove you dont actually have a lot of hands on experience ?
If you actually DO a synth, why not post YOUR data ?
Jared just copies and pastes. |
The answer is very simple- I made styphnic acid many years ago. I took the method from one Russian book in a library. The paper text with it was lost
many years ago. Now I found a description in Jared's book. I used a similar method, but I used H2SO4 + some nitrate instead of HNO3 for the second
stage.
Women are more perilous sometimes, than any hi explosive.
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caterpillar
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| Quote: Originally posted by hissingnoise | | Quote: Originally posted by caterpillar | | BTW, RDX can be prepared with the aid of the usual mixed acid. And mixed acid can be easily prepared if you have Ca(NO3)2. |
(Ahem!) Mixed acid cannot be used for RDX as H2SO4 decomposes hexamine ─ and why would you use calcium nitrate for
HNO3 when the sodium salt is less hygroscopic and so much more convenient?
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Yes, mate, this is what you may read in books. But there is a way to use mixed acid, however. Let's go.
ＣＨＩＮＥＳＥＪＯＵＲＮＡＬＯＦＥＮＥＲＧＥＴＩＣＭＡＴＥＲＩＡＬＳ Vol 16 No 1 February, 2008
Ｓｙｎｔｈｅｓｉｓｏｆ Ｋｅｔｏ ＲＤＸ ａｎｄｉｔｓ Ｃｈａｒａｃｔｅｒｉｚａｔｉｏｎｓ
Ｃａｌｃｕｌａｔｉｏｎ.
Don't be cofused by the word KetoRDX- this method gives the mix or KetoRDX and RDX. Not bad for a method, using mixed acid, eh?
Read this discussion: http://www.sciencemadness.org/talk/viewthread.php?tid=28395 you'll find many interesting there and when Ca(NO3)2 is better than NaNo3
Women are more perilous sometimes, than any hi explosive.
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kratomiter
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In my experience, picric acid is a pretty good secondary and the synthesis is easy. I always make it from aspirin and sulfuric+nitrate mix. The last
batch wasn't pure (more obscure yellow color), so be sure you get rid of aspirin's fillers, now I don't know how to remove impurities...
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caterpillar
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| Quote: Originally posted by kratomiter | | In my experience, picric acid is a pretty good secondary and the synthesis is easy. I always make it from aspirin and sulfuric+nitrate mix. The last
batch wasn't pure (more obscure yellow color), so be sure you get rid of aspirin's fillers, now I don't know how to remove impurities...
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It is better to make it from phenol- but if it is the problem, use aspirin.
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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| Quote: Originally posted by kratomiter | | In my experience, picric acid is a pretty good secondary and the synthesis is easy. I always make it from aspirin and sulfuric+nitrate mix. The last
batch wasn't pure (more obscure yellow color), so be sure you get rid of aspirin's fillers, now I don't know how to remove impurities...
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I used a sort of hybrid method, using 70% Nitric acid and since I was running low finished off with KNO3.
Very well behaved reaction, very good yields too.
second pic is 7 grams being converted to the ammonium salt that too went very smooth and easy
Aspirin is fine, wasting time to go all the way back to phenol offers nothing, so less you just happen to have crap loads of phenol laying about!
  
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kratomiter
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I don't have access to phenol, so I go with aspirin. I usually get very pure picric acid, I just screwed up the last synthesis in some step.
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Tkuze
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Aspirin extracted and deacetylated to salicylic acid, which is then used creates a much more impure product and tougher reaction than if buying pure
salicylic acid. The difference is evident in the sulfonation step, as the extracted and recrystallized salicylic acid/ sulfuric acid mix will form a
black solution. Pure salicylic acid/ sulfuric acie mix will form a beautiful magenta/ lilac color.
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caterpillar
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I used H2SO4 + KNO3 or NaNO3 instead of mixed acid. Both worked fine, but once I tried HN4NO3 and got lots of NOxes. The mix in my vessel became like
foam full of red gas, the vessel was overwhelmed and I had to interrupt the process.
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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converted my full batch to Ammonium Picrate. I added strong ammonium hydroxide till just slightly basic, then as it was fully dissolved adjusted to a
PH of close to 7 as possible, then boiled solution down.
then slowly allowed it to recrystallize over night, then left in fridge for the day.
[Edited on 7-6-2019 by XeonTheMGPony]
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caterpillar
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Look, Xeon, it can be done easier. Make slurry- picric acid plus some water, not much. Add in small portions NH4HCO3 (or (NH4)2CO3 ) and mix it, while
it is hissing. A small excess of carbonate is useful- no free acid. Then put the mix on fresh air and wait when it is dry. No large volumes of water.
Same way to make kalium picrate.
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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this served as the first recrystallization too, I tend to double up things to avoid excessive handling. there was a point to the method used.
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MineMan
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I don’t mean to be ignorant. But. Was Picric acid not an explosive of the very early 1900s, are there not better EMs with simpler OTC synthesis for
us clandestine to semi professional scientist?
I feel like I am missing something about the excitement of Picric... can some please correct me if I am wrong? Is it merely a curiousity if not used
for other EM synthesis?
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underground
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In my personal opinion you are right Mineman. I actually cannot see any reason why nitrating anything else rather than pentaerythritol. Best yields,
best performance and very good stability. Now if something else is going to be found that it can be easily made with OTC chemicals and it have good
performance, i will move into it. Most of us looking for something like that.
[Edited on 7-6-2019 by underground]
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Tkuze
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Mineman and Underground- I totally agree. There is only a historical appreciation for PA in my opinion and its a good starting point for EM. I sort of
disagree about PETN. I Find ETN more versatile and easily made. Its casting ability is probably its best aspect.
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underground
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I have both made and detonate ETN and PETN. From the 1st time i tested PETN, i have never made ETN again. I can achieve pretty high density with PETN
by pressing it. It is more powerful and i got better yields from the same acids. It is not that hard to initiate by shock and it is more insensitive
than ETN. I have calculate the cost of both ETN and PETN and despite E is cheaper than PE, it ends up PETN to be cheaper for me at least due to better
yields.
For the casting ability of ETN, i never cast it because i am afraid a bit 
Despite that, there is a topic about casting ETN/PETN mixture, it is even better than ETN itself, you should try it out.
[Edited on 7-6-2019 by underground]
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Tkuze
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Underground- I 100% agree, although I must add that I have observed several runaway pentaerithritol nitrations and only one with erythritol. Also PE
is much harder to find and suspicious. Erythritol can be bought at yiur local grocery or health food store. Try melt casting. Its relqtively safe. Its
been played with in molten form and its not super sensitive.
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Tkuze
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And yes, PETN yields are higher as well. Also ETN has a near 0 oxygen balence. I think its a very versatile, more available, easier compound in my
opinion. Its RE factor and velocity is similar. The best way to play with it is to put like 20g in a pill bottle and heat in water bath at 70C until
it melts ( takes some time), take out of the bath, let cool slightly until viscous and you can use a marker or plastic rod with the diameter of your
Blasting Cap to make a cavity. Add the BC when ready to use and you can keep it in the pill bottle and fill the rest of the empty space with cotton or
more 2°, or whatever the hell you want. Or you can remove and do whatever else you desire. The density of the MC is very high and avoids the risk (
albeit small ) with pressing.
Best use - wrapping your old college history notes and papers around 10g cast and watching it shred into a million pieces. 
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caterpillar
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| Quote: Originally posted by Tkuze |
Best use - wrapping your old college history notes and papers around 10g cast and watching it shred into a million pieces. |
Small piece of kalium picrate in your friend's cigarette.
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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| Quote: Originally posted by MineMan | I don’t mean to be ignorant. But. Was Picric acid not an explosive of the very early 1900s, are there not better EMs with simpler OTC synthesis for
us clandestine to semi professional scientist?
I feel like I am missing something about the excitement of Picric... can some please correct me if I am wrong? Is it merely a curiousity if not used
for other EM synthesis? |
novelty and an appreciation of Historic EM's
It was all so used as a burn dressing at 4% solution so it all so served as a ww1 medicine and dye
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caterpillar
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| Quote: Originally posted by MineMan | I don’t mean to be ignorant. But. Was Picric acid not an explosive of the very early 1900s, are there not better EMs with simpler OTC synthesis for
us clandestine to semi professional scientist?
I feel like I am missing something about the excitement of Picric... can some please correct me if I am wrong? Is it merely a curiousity if not used
for other EM synthesis? |
The story of PA is really interesting. It was., of course, an explosive- no matter. if someone knew about it or not. It was used, yeah, as yellow
paint and in medicine- to sterilize skin in surgery. Later it was used as explosive, but this usage met with real problems. PA is acid and makes
dangerous salts of iron for example. Its melting point is 122 Celsius- a hot water bath cannot be used to melt it. When it freezes, it significantly
decreases in volume, making cavities in shells. The inner space of shells had to be protected by pure tin without a significant amount of lead. Such
pure tin was a problem. Some people died, performing corresponding investigations. You definitely have no idea about Panpushko- the Russian
researcher, who died after an explosion in his laboratory. The Russian fleet was defeated at Tsushima and one of the reasons were shells- Japanese
ones were more powerful than the Russian ones. Russian used pressed NC, Japans PA. NC is more powerful, but it can't be pressed to 1.7 kg per liter-
only to 1.3. In shells, the volume of camor (the space for explosive) is strictly limited and explosive with a higher density is preferable. Well,
later TNT replaced PA, but for us, PA is much better, It doesn't require fuming sulfur acid for preparation.
Women are more perilous sometimes, than any hi explosive.
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Herr Haber
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| Quote: Originally posted by Tkuze | | Underground- I 100% agree, although I must add that I have observed several runaway pentaerithritol nitrations and only one with erythritol. Also PE
is much harder to find and suspicious. Erythritol can be bought at yiur local grocery or health food store. |
Chasing the runaway:
RFNA more yellow than red was used. It was slightly below 80%.
Under the same conditions on the same day with the same acids:
ETN went smootly between 5 and 10 Celsius.
1st PE ran away when I stopped paying attention for less than 5 seconds. I had to drown the mix.
2nd PE ran away while I was answering nature's call. It clearly showed it's intentions from the start so I was not surprised.
I agree with you 100 %
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underground
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I have never had any PE run away. I keep the temp below 10c when i add the PE, 15 minutes after the addition is complete i raise the temp to 60-70
slowly. Never had any issue and yields are pretty good.
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