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franklyn
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I like surprising quirky procedures. I think this is interesting.
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Motherload
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Does 68% HNO3 suffice for the above reaction ?
"Chance favours the prepared mind"
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Pulverulescent
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I'd doubt it, Motherlode ─ I'd guess >90%!
Do you have a lot of that old HMTD lying around? 
"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"
A Einstein
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Motherload
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Yeah it's fermenting in my wine cellar.
Well if one has to use WFNA ..... Why bother with the shitty >30% yield ?
Not to mention the need for me to wear a diaper when handling organic peroxides !!
Any input on my previous questions regarding mixed acid nitrations ?
Quote: Originally posted by Motherload  | Can one use a mixed acid nitrolysis of hexamine with nitrate salt and excess H3PO4 ?
I found a local chem supply for 85% H3PO4.
Or can one do a nitration of Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate with H2SO4 and nitrate salt ?] |
[Edited on 24-7-2013 by Motherload]
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Rosco Bodine
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There were some experiments done by Boomer looking at limiting ratios of acid to hexamine dinitrate for predictability of good yields.
http://www.sciencemadness.org/talk/viewthread.php?tid=4701&a...
Some discussion of reaction conditions and times and additives effect is found in the same thread.
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Vikascoder
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is this correct
| Quote: Originally posted by phantasy | Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205
as a dehydration agent . In 100ml HNO3 1.42gr/ml density, by 0cº temperature, in course of 10 minutes was slowly added 100 gramms of P205, then all
P2O5 was added, mixute was heat to 50cº to dissolve deposition, after temperature of reaction solution place at 0cº, 10g of hexamine was slowly
added in solution, temperature of solution was near 5cº. Solution was keep in 30 minutes, and add to 500 ml cold water with ice. This mixture was
filtered, deposition washed 3 times by 100ml of water and dry out. 13,9 gramms of RDX with 204.4cº melting poing was obtained, i have a photos of
product and another.
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Well the process I have ever found for making RDX uses HNO3 of >90% concentration and he have made RDX with HNO3 of 70% concentration only is this
data correct can RDX BE MADE WITH 70% HNO3 ONLY
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VladimirLem
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| Quote: Originally posted by Vikascoder |
Well the process I have ever found for making RDX uses HNO3 of >90% concentration and he have made RDX with HNO3 of 70% concentration only is this
data correct can RDX BE MADE WITH 70% HNO3 ONLY |
Its correct, but he used some extreme stong dehydrating agent (P2O5) to that 70% HNO3
Without that dehydrating agent it would take aloooot (~days) of time to get RDX and the yield would be extremely low - all in all: that wouldnt work
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malford
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Has anyone else tried this method? P2O5 is available for <$14 for 250g and 70% HNO3 is available for <$20 for a liter. This would be far cheaper
than producing or purchasing WFNA.
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roXefeller
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Bump
I didn't want to start a new thread on this when this one is relevant. How do the linear nitramines finish the polymerization into the cyclic trimer?
I can work out the nitrification of the hexamine, and the nitronium doing an excellent job and breaking the hexamine into linear nitramines. The
addition of urea nitrate and ammonium nitrate have a strong effect empirically on the result. I expect the species resulting from the decomp of
byproducts at higher temperatures plays a role also. It was mentioned that the ammonium salt might act as a catalyst (as it does in other reactions).
The Bachmann, et al article from 1951 regarding this used a nitrogen tracer and they indicated that a not insignificant portion of the ammonium ion
ends up in the final trimer, suggesting that it more likely makes up for the nitrogen imbalance in the hexamine. Would this indicate that a more
stoichiometric addition of ammonium nitrate is called for?
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roXefeller
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I found quite a discussion on nitramines in the Agrawal, Hodgson Org Chem of Exp text. It referenced the Bachmann results for increased yields using
NH4NO3 as well as pointing out the 3 and 4 nitrogen linear nitramines that form at low temperatures prior to the heterocycle forming. I'm going
through the Urbanski text still.
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roXefeller
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Quoting Agrawal:The nitrolysis of hexamine (104) is one of the most complex and widely studied processes in
the history of energetic materials synthesis. There are twelve CH2–N bonds in hexamine (104)
which can undergo scission, and with nitrolysis occurring to varying extents, it is unsurprising
that many different compounds can be produced during these reactions. Many of the possible
compounds are transient intermediates or are too unstable for isolation, as in the case of many
linear methylol nitramines whose existence is known from their reactions in solution or from
the isolation of their acetyl or nitrate ester derivatives. With so many reaction routes available
during the nitrolysis of hexamine it may seem strange that the cyclic nitramines RDX (3) and
HMX (4) can be isolated in such high yields. The reason for this observation is that both RDX
and HMX are very chemically stable and by far the most stable compounds present under
the harsh conditions of the nitrolysis. If fact, studies have shown that various fragments from
the nitrolysis of hexamine can recombine to form either RDX or HMX and so provide a sink
for active methylene and nitrogen containing fragments. Linear methylol nitramines and their
derivatives are unstable under the nitrolysis conditions and at reaction temperatures of 80◦C
they can fragment into smaller molecules which are also capable of forming RDX or HMX. End quote
I was a little disappointed with the Urbanski text. But I found the above quote on rereading Agrawal. It would seem that cyclic trimerization is
merely a product of the stability sink. The addition of AN to the mix then adds the necessary nitrogen to the soup that is already leading towards
stability in RDX. It does say to use a saturated AN / nitric acid solution as a nitrating medium at a temp between 60-80oC to prevent a hexamine
buildup. What is the solubility of AN in nitric acid?
[Edited on 23-12-2013 by roXefeller]
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Vikascoder
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What about the synthesis of rdx using other anhydrides like phthalic anhydride instead of acetic anhydride because phthalic anhydride is easily
available. Or the possible way of making acetic anhydride from phthalic anhydride
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underground
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I believe one of the easiest synthesis of rdx would be through the keto-rdx process with just only NA,SA,U and hexamine, and may the NA can be
replaced with SA/Nitrate salt. Check this pdf file
[Edited on 30-1-2014 by underground]
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Vikascoder
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| Quote: Originally posted by underground | I believe one of the easiest synthesis of rdx would be through the keto-rdx process with just only NA,SA,U and hexamine, and may the NA can be
replaced with SA/Nitrate salt. Check this pdf file
[Edited on 30-1-2014 by underground] |
In simple words I would like to tell you that rdx can not be made with sulfuric acid based nitrations do some research and then post on sciencemadness
threads
[Edited on 30-1-2014 by Vikascoder]
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underground
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With this way, it can...
Attachment: Synthesis+of+Keto-RDX+and+its+Characterizations+Calculation.pdf (1.1MB)
This file has been downloaded 980 times
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Motherload
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I was wondering about CH2Cl2 as a solvent during nitrolysis.
Since only anhydrous (covalent) HNO3 is soluble in CH2Cl2 ..... any diluted HNO3 (ionic) should phase separate from the solution due to the generation
of H2O when HDN is added. The dilute aqueous layer shouldn't interfere with the HDN and can be later recycled to produce more HDN.
This should keep the nitrolysis mix anhydrous and separate and shouldn't compromise yields.
Any thoughts ?
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TheAlchemistPirate
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Hey im posting this question here because I don't want to make a new thread and it seems relevant enough.
Is nitric acid produced by distilling KNO3 and H2SO4 (not vacuum) going to have more water in it than using maybe magnesium nitrate as it is
anhydrous? I haven't really seen any threads on this that came to a conclusive answer.
"Is this even science anymore?!"
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Turner
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No use 33ml:30g that is H2SO4:KNO3 for distillation of anhydrous nitric acid, this is a good ratio assuming sulfuric acid concentration is 95%+ and
your KNO3 isn't wet obviously.
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TheAlchemistPirate
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I meant anhydrous as in not making water when reacting with acids like sulfuric, I was led to believe that it could happen. But thanks, and sorry if
this isn't related to the thread.
[Edited on 28-3-2014 by TheAlchemistPirate]
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roXefeller
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This isn't acid/base neutralization where salt/water is created. This is a double replacement reaction. On that subject, never put a dry base into
conc. H2SO4, far too much energy release if not done well. The water that starts out in the reaction is the 5% of H2SO4, and the HNO3 will cling to
it azeotropically unless enough excess H2SO4 is present to dehydrate (hence the suggestion of 33:30 which has about 2:1 molar, one mole to react, one
to dehydrate). Water will later come from the distillation if the HNO3 starts to decompose at temperature, forming H2O vapor and NOx
non-condensibles. So you will generate diluent water.
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Vikascoder
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Well this thread have confused me a lot about the synthesis of rdx will anyone please help me with synthesis of rdx using hexamine dinitrate and
concentrated nitric acid 95+% conc and I don't have acetic anhydride
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TheAlchemistPirate
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This guy already showed a way. | Quote: Originally posted by lucifer | I’ve made rdx with distilled 99% HNO3 and with methenamine,
The Yeild wasn’t bad, 74% (29,7gr rdx out of 25gr methenamine).
I,ve changed the nitration time in meglomainia’s method, to get a better yeild.
(info from urbanski).
Slowly ad 25gr methenamine to the HNO3, which went quite easy keeping the temperature under 30degr C
After that put the solution in a water bath of 60 degr C, letting the temperature of the solution rise to 55 degr C Keep it at this temperature for 12
minutes.
Then cool it down in a ice bad to 20 degr C
During this phase some rdx becomes visible in the solution.
Let it stand for 10 min.
Then add to the solution 400 ml of ice water
A lot more of rdx will precipitatet out of the solution.
Let this solution stand for 5 minutes
After filtering neutralised the rdx with 400 ml 5% sodium bicarbonate solution.
The yeild after completely drying was 29.7 gr which is if I am ride about 74%
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Zyklon-A
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Can we please try and capitalize acronyms? (RDX) I mean, come on, here we are making high explosives. Lets try not to act k3wl. I know
TheAlchemistPirate, that you are capitalizing - I'm talking to those who aren't.
http://www.sciencemadness.org/talk/viewthread.php?tid=14999
| Quote: Originally posted by watson.fawkes | I suggest two social norms for capitalization. A social norm means that members may urge compliance independently, with requiring an official policy.
All chemical compounds should use proper element capitalization. I know what "naoh" probably refers to, and it's likely not a
misspelling of the guy with an ark. Nevertheless, it's still harder to read. My attitude, rarely expressed directly to members who do this, is "If you
can't be bothered to hit the shift key, I can't be bothered to care about your question."
All abbreviations should be spelled out in full at least once before they are used, especially in subject lines that open new threads and appear
on summary pages and in HTML titles. I suggest the spell-first, abbreviation-in-parentheses-following (SP-AiPF) convention for clarity. SP-AiPF is
pretty widespread already. My attitude, similarly mostly silent, is "If you can't be bothered to explain yourself, I can't be bothered to care."
To my mind, these are some of the least burdensome consequences of a general care in writing for many other people to read. There's already a
social norm here that members should at least some research before asking a question. How much less work is it to take an extra moment to ask a
question legibly? |
[Edited on 1-4-2014 by Zyklonb]
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underground
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Idea for simple RDX synthesis
I was wondering if RDX can be made by mixing H2SO4 with an excess of Ammonium Nitrate, so all of H2SO4 is going to react, to form
pure HN03, and also the rest AN is also going to help the formation of RDX
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DubaiAmateurRocketry
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^ RDX probably decompose in nitric acid which is whyyyy people use Ac2O and HNO3 for nitration of high yield.
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