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Tkuze
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General question about experience with picric acid
Obviously picric acid was a staple of militaries such as the japanese during the beginning of the 20th century.. and germany bought tons of aspirin
and salicylic acid pre-war from the US to manufacture it. My experience has been that although PA has a high value as an intermediate to picramates
and DDNP, but it seems useless as a secondary. Even testing using an improvised #8 cap seems to not do much. Theres always a sort of mist of yellow
and mild DDT, whereas replacing the PA with a nitrated polyol works magnificently. Priming mixture:lead styphnate 200mg, primary: lead azide
(dextrinated; 90mg or pure; 70mg), Secondary:700mg pressed + 300mg lightly pressed ETN, PETN, MHN, RDX MIX(50/50 with ETN to improve sensitivity).
This works excellent, but looking back at the first compound made which inspired curiosity in this field, picric acid, I wanted to use my experience
to test its effectiveness again
Its seems to not be bery good at all, besided staining everything. Even in combo with melt casts, it seems to have a negative effect. What do you
guys think? Assume I havent been doing anything right
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Herr Haber
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Nitrated polyols dont require the same level of confinement to impress you as PA does. Also, they tend to have a higher RE than picric acid.
I can only assume you got that "yellow mist" because some didnt go DDT.
Only suggestions I have is to use a stronger confinement and find every topic about the subject where Rosco contributed. His words are gold (when it
comes to picric acid).
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Tkuze
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Thanks man. I was curious because its used so commonly when you watch WW1 and WW2 documentaries and seems inneficient. hey usually combine it with TNT
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hissingnoise
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Though PA is more sensitive than TNT ─ it has better OB, brisance and power than that compound.
Its acidic nature and relatively high sensitivity were the factors that militated against its wider acceptance after WW1...
It was said that because British PA-filled shells exploded on impact with armour, whereas German shells with TNT could penetrate armour before
detonating, the British lost more ships and men than did the Germans in the battle of Jutland.
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Tkuze
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Thats a very good point. The coolest thing in WW2 is the use of HMX in the fat boy as the uranium slug propellant. Are there any methods to produce
HMX without Acetic Anhydride?
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underground
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Quote: Originally posted by Tkuze  | | Thats a very good point. The coolest thing in WW2 is the use of HMX in the fat boy as the uranium slug propellant. Are there any methods to produce
HMX without Acetic Anhydride? |
Synthesis of DPT ftom hexamine then nitrate the DPT with FNA.
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caterpillar
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Kalium picrate explodes been ignited in confinement. No need in the detonator. I initiated mixed AN+ammonium picrate, a mix that is obviously less
sensitive than pure picric acid, with the aid of 0.5 gr TATP.
Women are more perilous sometimes, than any hi explosive.
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NeonPulse
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It sounds like you have not fully nitrated the Precursor. In my opinion Picric Acid is very powerful and a worthy secondary. I had this problem with
the yellow cloud and little damage to test plates and reworked my procedure to produce a very pure product with all the desired properties. It’s
probably the most versatile explosive you can synthesise as it is a precursor itself to many other interesting explosives. I’d say almost perfect-
except for the yellow staining it leaves everywhere.
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caterpillar
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| Quote: Originally posted by NeonPulse | | It sounds like you have not fully nitrated the Precursor. In my opinion Picric Acid is very powerful and a worthy secondary. I had this problem with
the yellow cloud and little damage to test plates and reworked my procedure to produce a very pure product with all the desired properties. It’s
probably the most versatile explosive you can synthesise as it is a precursor itself to many other interesting explosives. I’d say almost perfect-
except for the yellow staining it leaves everywhere. |
Probably, you are right. I read about a simple test-
0.5 gr in tinfoil on a steel plate. Strong impact with hammer must cause an explosion if not-you have a mix of dinitrophenols.
Women are more perilous sometimes, than any hi explosive.
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NeonPulse
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But even the Hammer test here isn’t reliable. I’ve made some incredibly pure picric acid before with huge well defined crystals almost clear and
although it detonated powerfully confined and provoked with some Lead Azo -Clathrate, it took several very solid whacks to set it off. Often just
pulverising it.
The times it did go off though, it was loud and plenty of orange sparks with the telltale smell.
It’s obvious but In my opinion The only way you can truly tell the purity is to run a known synthesis, carefully, with known parameters leading to
predictable product.
By far The best method I’ve found uses NaNO3 and was developed
by Rosco Bodine.
I did a video of
https://m.youtube.com/watch?v=7es7kMAZyFY&autoplay=1
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Tkuze
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I am really convinced that the product is fully nitrated. I have used multiple procedures and settled on the best of all combined. Do you have any
specific advice to improve synthesis, like using pure acids? I am positive it is pure because it was used for DDNP and the product was pure.
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Tkuze
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Also, I have watched that video many times, but I never used nitrate salts. I used highly pure nitric acid
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caterpillar
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Nitrates, dissolved in the conc H2SO4 are more powerful nitrating agents, than the usual mix of HNO3+H2SO4. I described once the method that U used.
250 gr of phenol + 800 gr of H2SO4 94%. I used a hot water bath but found that is is not necessary. 1000 gr of KNO3 + 1600-2000 gr of H2SO4. Both
solutions must stay for a night. Next day slowly add phenol, dissolved in H2SO4 to nitrating mix. The process takes hours- do not let the temp leap
up, try to keep the room temp or slightly above it. Then mix must stay for one night more. Next day slowly increase temp up to 100 Celsius by means of
boiling water bath. Keep mix at 100 Celsius for one hour. Then pour it into large enough volume of cold water with crushed ice. Filter yellow crystals
and wash them with a small amount of cold water. Oh, and if you wanna make some salt, do not dissolve it into the water. Add a small amount of water
and mix slurry with K2CO3, NH4HCO3 and so on.
Women are more perilous sometimes, than any hi explosive.
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Tkuze
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Thanks. I will give it a try using salicylic acid. I want to just compare to synthesis of stypnic acid. During both synthesis, adding H2SO4 and
starting material and heating for 30-60 min results in both solutions becoming a lilac colored mixture, which is cooled and then nitric acid is slowly
added with heavy stirring and then heated up slowly to 90-100C and heated for 1h, where a large amount of bubbling occurs and then bright yellow
precipitate forms. This is heated for an extra hour or two and excess nitric acid or salt is added to ensure nitration. In the case of styphnic acid,
an eggshell white compound is isolated. This is added to an equimolar solution of NaOH until fully dissolve and solution is red. Lead (II) nitrate is
dissolved in H20 and kept at 65C. The stypnate solution is added dropwise while warm over several hours, resulting im a yellow or orange precipitate.
Nitric acid is slowly added at the end of reaction to turn the yellow precipitate dark orange/red. This is filtered and washed. Once dry, it is a very
powerful and sensitive priming mix. This is definately trinitrated. Basically same procedure as picric acid. And the styphnate is definately the
corret lead salt. But ill try your procedure. And buy phenol
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caterpillar
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I made styphnic acid, but the first attempt was not successful. I tried to make is just as I made TNP, but when I had placed resorcinol into H2SO4 it
turned into some stone. I made it via nitroso derivative- the first stage is the reaction of resorcinol with nitrite and diluted H2SO4, the output is
brown powder. The next stage is the reaction with diluted HNO3- sorry, I do not remember all details. But I made it.
Women are more perilous sometimes, than any hi explosive.
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caterpillar
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Taken from Jared Ledgard: Step 1: Preparation of Dinitroresorcinol monohydrate
Procedure:
To 16 liters of water add and dissolve 440 grams of resorcinol, and then 452 grams of 98% sulfuric acid. Immediately
thereafter, add 6800 grams of crushed ice to mixture, and then stir the mixture vigorously until the internal temperature of the
mixture reaches about 0 Celsius. Then prepare a solution by dissolving 600 grams of sodium nitrite into 3200 milliliters of
water, and then add this sodium nitrite solution to the sulfuric/resorcinol mixture over a period of 6 minutes while vigorously
stirring the mixture and maintaining its temperature below 5 Celsius. After the addition of the sodium nitrite solution, continue
to stir and cool the reaction mixture below 5 Celsius for 30 minutes. Note: A precipitate will begin to form. After the 30 minute
period, filter-off the precipitated dinitroresorcinol monohydrate, and wash with several hundred milliliters of cold water (use
gravity filtration).
Step 2: Preparation of Styphnic acid
Place 3000 milliliters of 40% nitric acid into a beaker, and then gently heat this mixture to about 30 Celsius. Thereafter,
carefully mix the moist filter cake, prepared at the end of step 1 to the nitric acid solution over a period of about 30 minutes,
while stirring the nitric acid and keeping its temperature around 30 Celsius. Immediately after the first addition of the filter
cake, nitrogen oxide gases will be evolved, followed by the formation of a foam (the foam will dissipate after about 10
minutes). After the addition, raise the temperature of the mixture to 95 Celsius, and then hold this temperature for 1 hour. After
heating for 1 hour, remove the heat source and allow the reaction mixture to cool to room temperature. Note: A precipitate will
form. When the reaction mixture reaches room temperature, filter-off the precipitated product, wash with 300 milliliters of 2%
nitric acid, and then with 600 milliliters of cold water. Then vacuum dry or air-dry the product. The result will be pale yellow
crystals, well suitable for use in preparing lead styphnate, or styphnic acid compositions.
At this stage you may use H2SO4 + some nitrate instead of HNO3
Women are more perilous sometimes, than any hi explosive.
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hissingnoise
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Oh no, not Jared Ledgard! Aaarrrggghhh!!!
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Tkuze
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Thanks for the procedure. Ill try it small scale. Im curious what your opinion is on the product originally described in this thread. The lead
styphnate currently is placed on a metallic spatula and a flame is slowly introduced from below, resulting in immediate DDT.
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caterpillar
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Yeah, mate, I share your opinion about dear Jared. But I originally took this "recipe" from the other book. And I made styphnic acid, using this
method- I only used H2SO4 + KNO3 instead of pure HNO3.
Women are more perilous sometimes, than any hi explosive.
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caterpillar
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| Quote: Originally posted by Tkuze | Thanks for the procedure. Ill try it small scale. Im curious what your opinion is on the product originally described in this thread. The lead
styphnate currently is placed on a metallic spatula and a flame is slowly introduced from below, resulting in immediate DDT.
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My opinion on picric acid is that it is excellent secondary- simple preparation, just for beginners. And some of its salts can be used instead of pure
TNP. I love it. Nice color, like pure gold.
Women are more perilous sometimes, than any hi explosive.
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Tkuze
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Ok thanks. Ill remove my bias and retry it and report back
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caterpillar
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Go ahead. I think (but it is the only my proposition) that one can use TNP for blasting caps. 1-2 gr of pressed TNP and 0.5-0.8 gr of lead picrate
above.
Women are more perilous sometimes, than any hi explosive.
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Herr Haber
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I'll stay biased towards that guy.
Let's not even point out his many mistakes. But how are you going to trust someone feeding you a synthesis as if it were a cooking recipe if he didnt
even try it in the first place ?
Who's gonna believe the guy nitrated 250 grams of phenol like described above ?
What now ? 16 liters of water ?
Looking for lab procedures I dont see the interest of (old) semi industrial method.
Burn this guy's books and get Urbanski instead !
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caterpillar
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| Quote: Originally posted by Herr Haber | I'll stay biased towards that guy.
Let's not even point out his many mistakes. But how are you going to trust someone feeding you a synthesis as if it were a cooking recipe if he didnt
even try it in the first place ?
Who's gonna believe the guy nitrated 250 grams of phenol like described above ?
What now ? 16 liters of water ?
Looking for lab procedures I dont see the interest of (old) semi industrial method.
Burn this guy's books and get Urbanski instead ! |
??? 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.
Women are more perilous sometimes, than any hi explosive.
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Tkuze
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Haha, I never use and probably wont use nitrate salts. Just pure Nitric acid
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