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Author: Subject: possible nitrations through h2so4/kno3
prometheus1970
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shocked.gif posted on 12-6-2010 at 13:26
possible nitrations through h2so4/kno3


At the risk of totally revealing my limited experience in this field,I recently discovered the production of nitric acid through sulfuric acid and a nitrate salt for the purpose of producing nitrated compounds (in particular etn, nitrocellulose) I've been working (without success as of yet with 98% H2SO4 and KNO3. I've been going strictly by the syntheses outlined that I've found, as I don't have the chemistry background to extrapolate the necesary formulae for what I want to do. I'm very interested in etn because it packs enough punch to be interetsing, but is insensitive enough that reasonable caution will prevent accidental detonation. I'm fascinated by chemistry, but have not yet had the chance to study it properly because I hold liberal arts degrees (psychology and philosophy) and didn't really need any science for BA's in those humanistic disciplines. But I digress. I'm wondering what kind of ratios of the two acids (HNO3 and H2SO4) you get when producing nitric acid in this matter. I also wonder what other primaries can be produced this way. Several other nitrated compounds (tnt egdn, ng) require the use of bona fide nitric acid rather than making it from a nitrate salt and sulfuric acid. I don't want to be spoonfed, just hoping someone could point me in the direction of getting the information I seek without having to get a master's degree in chemistry. I thank you in advance.

[Edited on 6-12-2010 by prometheus1970]

[Edited on 6-12-2010 by prometheus1970]




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[*] posted on 12-6-2010 at 16:52


Hippy willing to make exlosives ;-?

Other's will probably lay crap on you becouse opening new thread on things everyones knows how to do.
Just use search engine or go to youtube,there are some great videos that explain you,step by step what to do.

ETN is not something you wan't to start with,for example you don't even need concetrated,if any HNO3 to make ETN,
just use nitrate salt (KNO3 or even better NH4NO3 and H2SO4),it is not "reasonybly stable"
try wiht extra safe AN or wery small quanitities of AP or HMDT first,
try some low explosives mixtures before jumping on the high explosives just to get feeling how to handle them
and learn how important ratios really are in chemistry.

You need to UNDERSTAND what are you doing,it is not cake that can go dry or burnt,that goo-thing right there in that
little glass baker you are mixing is willing to end your life in no time!

Learn some stoichiometry,it is the boring part of chemistry bot once you know it is like riding a bike,
you need to learn how to calculate in moles(ammount of particles) if you are going to do ANYTHING.

Use other people recepies with caution and examining.

I know this tread goes to detrius,but hope I saved you at least a limb.
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prometheus1970
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[*] posted on 12-6-2010 at 17:51


I thank you for your candor. ETN is not my first attempt. I've been making black powder, flash powder (both with KCLO4 and KMNO4) as well as recrystallised sugar propellant. Perhaps I was led astray, but where I discovered etn it was described as a good synth for those trying to learn. I did have enough sense to avoid the organic peroxides, though they seem fairly straight forward. I don't want to mess with anything as sensitive as tatp or hmtd and I like that you can initiate etn with flash powder. I know not to use HNO3 for making etn, but isn't that just what mixing H2SO4 and a nitrate salt does? I kinda understand why you called me a "hippie", but you're not quite on the mark I'm still just this side of 40 years old (too young for true hippie) and I don't espouse any of the hippie ethos. I majored in psychology to earn a living (didn't work out that way) and double majored in the philosophy because it's that kind of analytical thinking at which I excel. Once again I thank you for your time and warning, it never hurts to be reminded that this hobby can be a hazardous once. Am I wrong in thinking of etn as being safer that the organic peroxides? I know it's not as insensitive as many of the AN compounds, but I like that if I scrape it off a wooden table with an index card (once powdered) it won't detonate before I have a chance to grab my ankles.



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[*] posted on 12-6-2010 at 19:37


@prometheus1970: If you ever find "recepies", make sure they weren't written by mfilip62. With this spelling there's probably something wrong with his "recepie" and it may cost you a limb ;)
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[*] posted on 13-6-2010 at 03:52


Quote:
. . . it's that kind of analytical thinking at which I excel.

Then you'll have no trouble finding the info you want in the ETN and other threads. UTFSE!


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prometheus1970
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[*] posted on 13-6-2010 at 13:15


I have been "u2uing", with him, he just pointed me to the preparatory manual of explosives. I generally try to avooid any synth referred to as a "recipe" regardless of spelling. To me that would be like taking my car to a mechanic who referred to the tranny as, "the gear changer thingie". Do you feel the preparatory manual of explosives is reliable?



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[*] posted on 13-6-2010 at 15:32


The preparatory manual of explosives is FILLED with mistakes and false patents. The group here once did an unofficial "count" as to how many mistakes and false patents were written in both the 2nd edition and 3rd: there were PLENTY of MAJOR errors. Indeed some were simply unworkable and false (see copper fulminate.....).
The book is not totally worthless but it is very dangerous to those who cannot substantiate the "shit from the Shinola" (feces and a buffing compound).




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[*] posted on 13-6-2010 at 18:21


Thanks for the heads up. I should know better than to look for a nice, tidy packeg with all the stuff I want to know about the chemistry of energetic materials. The main thing I got from him is that my powerful fear of organic peroxides may not be copletely warranted. I don't have an irrational fear of them, but everytime I see a synth for ap, hmtd or mekp, they always begin with, "do not try this unless you have experience with these compounds" it is very dangerous. I know that they can be very dangerous, but with due caution, I think it can be done safely. It's not like I chose tatp as the first thing I ever tried to synthesise. Today's internet is so universally accessible that there are plenty of people whoknow as little as I do (or sometimes less), but see nothing wrong with leaving their viewers/readers with the impression that they are experts. orting past those yahoos is what puts me in the position of trying very little due to preferring to err on the side of caution.



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[*] posted on 14-6-2010 at 01:37


Think Picric Acid: the beautiful nitroaromatic! PA has a brilliant and admirable character. As a first synthesis it has the pleasant expectation of being not too difficult and yet not altogether easy. Apart from the risk of inhaling nitrogen oxides that may be produced during synthesis, PA synthesis is very tame as far as explosion risk is concerned, even if a runaway reaction occurs. ( Runaways involving several thousand grams of reactants simply burst into flames and burn off quietly, no detonation.):P

Synthesis aside, Picric Acid has such astounding stability and utility that its applications and importance are decidedly striking. Surely it would be one of the most suitable for a first synthesis of a pure compound energetic material.:D

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prometheus1970
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[*] posted on 14-6-2010 at 10:05


Thanks. I'll look into TNP



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[*] posted on 18-6-2010 at 07:51


No no no Mr. Prometheus.
Picric acid is no good choice.
I would say ETN is a great choice.

I rub the course crystals between my fingertips while still wet and play with it till absolution comes....:D

No, really, ETN is not a bad choice to start with.
There are no complications of sensitive picrates and complexes forming.

You just have to treat it with respect, say like you would treat TATP or MEKP ( not suggested).
And please avoid that red gas (accompanying PA synth).
Shes a real bitch, not to be trifled with!

BTW, why not try out PETN?
This is THE best in my opinion.
It was my first ever synthesis and no complications arose.




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[*] posted on 18-6-2010 at 09:30


For every 10 synth. you found in the net,5 have seanse,
and probably one or to is doable.
I recommended Prometheus that book because it deals extensively with simple lab techniques in intro,I never said it is totaly realible.

I agree that PETN is far best, but you can't always choose, not anyone can find all the chemicals needed.

For example my first HE's were AP,MEKP and NG and I didn't hurt myself because I RESPECTED those substances.

TNP is interesting explosive and everyone who dares to call himself an "pyro" must make it sometimes :D
But it it too damn domplicated and dangerous for someone who never did anything in the lab and irresponsible to recommend it to the total amateur.
Noxious NOx fumes, full glass of hot concentrated acids
poisonous compound that stains EVERYTHING for weeks and makes pesky salts,
and not even mentioning insane water salability that can decrease yield.

Now excuse me,I must go to the firework festival!
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[*] posted on 18-6-2010 at 13:10


Thanks for the recommendations, but I have reasons for choosing the etn synth. 1.It seems straightforward enough for someone still learning this hobby. 2. it seems safe enough for the same reasons. I don't have the equipment for separating liquids (like mekp, ng, etc.+ cash is too tight for buying more stuff right now)3. can't find pentaerythriol without having to buy 100+ pounds of it4. phenol is another chem I don't have or have money for. m BTW I tried another etn synth today with what appear to be great yields (don't know for sure, it's neutralizing right now) I'll recrystallize it tomorrow and post hopw it all went. Thank you everybody that helped!



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[*] posted on 19-6-2010 at 05:25


You don't need phenol to make TNP,you can make it MUCH faster and easyer with ASA(from Aspirin)
Hope you made a good batch!

For example,there is no way I can make ETN because there is no erythritol where I live.
Closest thing you can get here is sorbitol in diabetic food stores.
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[*] posted on 19-6-2010 at 15:41


I found the erythritol from an online health food store. I read about a tnp synth using ASA, I'll have to try it once I get some denaturd alcohol (which I need to recrystallize the etn anyway). My last batch of etn was in the neighborhood of 27 grams from 15 grans erythritol. My main question for this thread was what all nitration processes can be done with h2so4 and a nitrate salt in place of h2so4 and hno3. I believe it can be done with nitrocellulose, but like ng, mhn and many other nitration reactions require hno3 for the process to work. I vaguely understand that mixing h2so4 and a nitrate salt sort of makes a sulfuric acid/nitric acid mix, but I also understand it's not that simple.



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[*] posted on 20-6-2010 at 03:43


@Prometheus.Check the freezing temp of HNO3.This is just a clue...Freeze that bitch out my friend.:cool:

[Edited on 20-6-2010 by Rain]




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[*] posted on 20-6-2010 at 05:03


Who saids you need denaturated alchohol!?
You can use acetone for extraction of ASA,actually you can use pretty much anything,even water.
It is bitch to find denaturated EtOH in USA compared with isopropyl(here is different)
Look in your inbox,I send you great synth. that really works.
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[*] posted on 20-6-2010 at 06:19


@prometheus1970 : I would strongly suggest you to start with other aspects of chemistry than making explosive compounds. A nice suggestion from my side is to try to make and isolate copper(II) chloride, using stuff you can find in hardware stores, drugstores and groceries. While doing so you need to do some research, you have to find some suitable reagents, need some glassware and need some theoretical background. Once you have succeeded in making and isolating some CuCl2.2H2O you will have learnt a lot, you will have collected some basic glassware, and the whole subjest of chemistry will be much more rewarding to you. And all this learning can be done safely without the risk of maiming or even killing yourself.

What you want now is like running, while you did not even acquire the capability to walk.




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[*] posted on 20-6-2010 at 07:17


Quote: Originally posted by woelen  
What you want now is like running, while you did not even acquire the capability to walk.
I think perhaps a more appropriate analogy, apropos more widely than just the present one, is that they wish to fly and all they're capable of now is jumping off a cliff.
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[*] posted on 27-6-2011 at 06:18


ETN, (KNO3+H2SO4+erythritol)
TNP, (KNO3+H2SO4+ASA)
PETN, (KNO3+H2SO4+Pentaerythritol)
HDN, (NH4NO3+HCl+mehanmine)
MHN + SHN, (KNO3+H2SO4+Sorbitol or Mannitol)
EGDN, (KNO3+H2SO4+ethylene glycol)
Nitrocellulose, (KNO3+H2SO4+cotton)

[Edited on 28-6-2011 by KING-pyro]
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[*] posted on 27-6-2011 at 12:51


The bottom line is you can nitrate nearly anything with KNO3+H2SO4 except some things that are too dangerous to do it that way... Eg: Methyl Nitrate, and some that are too finicky in their synthesis... RDX, PETN...

The proper ratio's are...
30g/100g Nitrate Salt/H2SO4(93%)
30g/91g Nitrate Salt/H2SO4(98%)

Those ratio's are proper for nearly all nitration's. I would suggest you keep nitration temperatures strictly at 15-20C and just dump them in water if they go over 25C... Until your experienced.

[Edited on 27-6-2011 by freedompyro]
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[*] posted on 27-6-2011 at 18:54


Quote:
The bottom line is you can nitrate nearly anything with KNO3+H2SO4 except some things that are too dangerous to do it that way... Eg: Methyl Nitrate, and some that are too finicky in their synthesis... RDX, PETN...

The proper ratio's are...
30g/100g Nitrate Salt/H2SO4(93%)
30g/91g Nitrate Salt/H2SO4(98%)

Those ratio's are proper for nearly all nitration's. I would suggest you keep nitration temperatures strictly at 15-20C and just dump them in water if they go over 25C... Until your experienced.

[Edited on 27-6-2011 by freedompyro]



I use different ratios in my nitrations. Where are you getting these numbers? I use ~32g KNO<sub>3</sub> to 50ml of 98% H<sub>2</sub>SO<sub>4</sub> when making cellulose nitrate. Also, the TNP from ASA synthesis ~ 1.8g per 4ml of 93% acid. (Rosco Bodine's workup, which I find gives superior yields when working from acetylsalicylic acid.)

I don't think that setting a standard ratio for all nitrations is wise. What is the scientific basis of your ratios? Are they purely based on your personal trails?

Also, not all nitrations need to be ran at reduced temps. I believe it depends on the site of the esterfication For instance, in the TNP synth described, heat must be added to the system to complete the nitration. Still, accurate temperature monitoring is vital when producing any nitric esters for safety.

Please don't make sweeping generalizations about these things. Proper research is necessary in this work. Using a set 'recipe" is dangerously lazy.

[Edited on 28-6-2011 by Bot0nist]




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[*] posted on 27-6-2011 at 23:32


Quote: Originally posted by Bot0nist  

I use different ratios in my nitrations. Where are you getting these numbers? I use ~32g KNO<sub>3</sub> to 50ml of 98% H<sub>2</sub>SO<sub>4</sub> when making cellulose nitrate.


Converting your numbers to weight. Your using 32g/92.5g. Assuming a multiplier of 1.85 for H2SO4 converting from volume to weight.

This ratio works perfect for everything from NG, ETN, EGDN, NC, and etc... It's also simpler to remember... 1/3 Ratio. :) People are rarely going to be nitrating something that doesn't use that ratio...

[Edited on 28-6-2011 by freedompyro]
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[*] posted on 28-6-2011 at 04:50


Lol, sorry freedompyro. I was seeing ml for the acid for some reason.



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[*] posted on 28-6-2011 at 08:04


The responses you have received are very wide ranging. It does not make then "bad or good"; but it does give to a very powerful illustration as to what you may need to help you learn. Science is similar to music in that practice and basic understanding is the hallmark of a usable understanding of the principal.
Start at the beginning. Learn why a deflagerrant would burn without external oxygen sourcing, eventually learn what takes place via a classic synthesis on a molecular level. The "Lab" has a very important place in this understanding but it's almost useless unless you understand why - what you are observing takes place. Reading and studying are infinitely more important than physical preparation at a entry-level learning stage. They prevent negligence and they maintain a cogent understanding of why something tales place.
Why someone understands WHY something takes place they can delve further into it with a grater perception of it's utilitarian value. We "walk before we run" so that running provides depth to the passing world around us (and so we don't fall, as well!)

Anyone can follow a "recipe", yet the actual learning is missing if we don't know WHY something is taking place. Take advantage of all the material within this Forum. You could literally spend a great deal of time answering you own questions and finding ways and means to get a better grasp on what makes sense to you in the context of your curiosity.

Detonation is fascinating. It is also very complex in what is actually taking place on a molecular level. These issues are MUCH more appropriately met through STUDY rather than making noise (much safer also). Frankly there are things about the physical sciences that make seemingly dull subjects come alive. But they require that the student pursue them. Do you absolute best NOT to take short-cuts. Just like music, the really well versed pupils have patience....not only with the subject, but with themselves.



[Edited on 28-6-2011 by quicksilver]




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