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PerFecTioNisT
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C.T.M.T.N.A (R-salt)
I.m intresting about this HE, and maybe there are people who did this explosive by this recept?
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This is R.D.X., but missing three oxygen atoms (one from each NO2 group). It uses no concentrated nitric acid. The only acid used is hydrochloric, and
it doesn't even have to be very concentrated. This explosive is carcinogenic and toxic, contact should be avoided. However, this is perhaps the
best explosive to make at home since it is easy to produce and powerful. The reason it's not used militarily is the low yield of 30% (I have seen
50% stated, but this means that the weight yielded is 50% of the weight of hexamethylenetetramine used, e.g. 3.5 grams of C.T.M.T.N.A. from 7 grams of
hexamethylenetetramine.)
VoD is 7800 m/s at 1.57 g/cm3. Relative briscancy is 1.17. Lead block expansion is 370 cm3. At this density 2.5 grams of Mercury Fulminate will cause
detonation, at 0.85 g/cm3 a mere 0.3 grams of Mercury Fulmiate will suffice!
You will need:
7g of hexamethylenetetramine,
60mL of 15% hydrochloric acid,
10.5g of sodium nitrite,
Distilled water,
50mL of 10% sodium carbonate solution,
20mL of acetone,
1g of sodium carbonate,
An ice bath,
A 150mL beaker,
A thermometer,
A filter funnel,
Three filter papers.
1) Dissolve the hexamine in 25mL of water and add the hydrochloric acid in the 150mL beaker.
2) Cool this to 0*C in the ice bath, and add a solution of the sodium nitrite in 50mL of water, while stirring.
3) Leave the solution to react overnight at 5*C, and then filter out the crystals.
4) Wash them with 200mL of water, then the sodium carbonate solution, then another 200mL of water.
5) Dissolve them in the acetone at around 40*C, add the 1 gram of sodium carbonate, and stir for 5 minutes.
6) Filter the solution
7) Dump the filtrate into 100mL of cold water in the other 150mL beaker to precipitate the crystals.
7) Filter them out, and leave them to dry in a warm, dry place in a thin layer.
Who had try to do this?
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Mumbles
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I've tried it and gotten shit for results. I keep the temp low, but it started bubbling. It's definatly not ammonia, or formaldehyde or
HCl. It's hard to explain. It smells kinda like warm bread if that makes any sense.
After maybe 45 minutes this foamy stuff on top forms. I think this is the R-salt. I let it react for the time recomended by Mr. Cool, and by morning
the foam was all but just about gone. I don't like it. I would be willing to try if I found a better method.
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chemoleo
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Federoff R-Salt Preparation
Well I didn't realise how remarkably simple the synthesis is. Indeed, acc. to Federoff, only the pH seems to influence nitrosylation. The lower,
the better essentially, else one gets di-nitroso products. At pH 1, one exclusively gets the trinitroso form.
In fact, this is the optimised prep in Fedoroff:
Bachmann & Deno (Ref 6) added simultaneously a soln of NaNO2 in 6M HCl,
at a rate required to maintain a pH of 1, to a solution of hexamethylenetetramine in ice & water. The mixture was held at 0° for 30 minutes. The
yield of practically pure product was 50% (mole for mole basis)
Maybe this ought to be done that way instead.
[Edited on 22-2-2005 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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PerFecTioNisT
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No product..... :(
I didnt keep the temperature when added NaNo2 soak, when I added it, all stuff started bubling and was brown fumes, its no2 if I dont wrong.But
tomorow i did not saw any cristals.....What was wrong?NO product?
[Edited on 23-2-2005 by PerFecTioNisT]
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Mumbles
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Is that reference saying a solutions of NaNO2 and 6M HCl added simultaniously, or a solution of NaNO2 in 6M HCl. The simultaniously would make me
think that it is 2 separate, but it mentions a singular solution and uses "in".
I may try out the ice directly in solution next time. It seems that would work a lot better for cooling.
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chemoleo
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Well I copied it straight from Federoff, no rewording. If you really want to be sure, I guess you ought to get that reference.
The way I understood it is that you mix NaNO2 with HCl, icecold, so as to prevent NOx evolution. This you add to the hexamine.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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PerFecTioNisT
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Yesterday I did one more.I cooled my stuff to -2C and added nanao2.The highest temperature was 10C, al stuff bubling and I let him to stayed in the
yard over night.And this morning i didnt find the product  I dont know what to
do......
And what is the Federoff?Maybe there are several recept to do this R-salt?
[Edited on 24-2-2005 by PerFecTioNisT]
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stygian
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To me it's saying the hexamine and HCl are in one beaker, cooled to 0c, then NaNO2 solution is added.
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J_O_H_N_Q
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referencing
Hey Perfect, nothing personal man, but, shouldn't you at least tell people that you quoted Mr Cool's webpage?
He did go to all the effort to write that stuff up, at least give him credit for it.
[Edited on 2-3-2005 by J_O_H_N_Q]
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PerFecTioNisT
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Yes this is from MR.COOL web , soory...I think that all peoples knows.
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SAM4CH
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Oxidize R-Salt!
Can I convert R-salt to RDX?! more details!
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Pyro_boy
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C.T.M.T.N.A (R-salt)
C.T.M.T.N.A (R-salt): Actually the yields can be much better if your using Muriatic Acid, 31.5% HCl and potassium nitrate.
I've gotten up to the high 60% yeilds with this method. i'm going to tweek the formula and see if 80% is possiable.
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chemoleo
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Potassium NitrAte?? 
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Pyro_boy
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yeah, It was suppose to be Nitrite, but I used Nitrate instead. I worked, oddly. NO3 instead of NO2..
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The_Davster
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You probally just have HDN...
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Esplosivo
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I don't understand the exact mechanism by which this reaction proceeds, but mixing a nitrite with hydrochloric acid clearly indicates the
formation of nitrous acid. I would say that what occurs is a sort of nitrosylation, but I am not sure. If this is so, it surely would not give the
same results if the nitrite is replaced with a nitrate.
Theory guides, experiment decides.
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sparkgap
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Just my two cents, but the guy made no mention of testing his purported product chemically to verify it was the subject explosive. So we can't
really say if it was. Most likely, however, would be that something structurally different, but just as explosive as the original, was made.
sparky (^_^)
"What's UTFSE? I keep hearing about it, but I can't be arsed to search for the answer..."
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Axt
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| Quote: | Originally posted by Rosco Bodine <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=3033">here</a>
Also hexamine or hexamine dinitrate or even HMTD could form R-salt or a similar derivative . (from NOx) |
I'd previously tried to get R-salt by bubbling N2O3 through 20g hexamine, 100ml 32% HCl and 150ml water, cooled to 5°C. A precipitate did seem
to form (solution turned white/turbid) but temperature gets out of control and solution fumed off as you get if r-salt is added to hot acid (its not
stable in acid solution, far worse if its hot). If one was going to attempt this you will need to use a slurry of crushed ice, external cooling wont
work.
Anyway, heres conventional r-salt through NaNO2/HCl/hexamine. Three solutions were made, one containing 60g 35% HCl in 100ml water, one containing 40g
NaNO2 in 80ml water and one containing 20g hexamine and 60g HCl in 100ml water. The NaNO2/HCl solutions are combined, producing blue solution of
nitrous acid. This is then added to the hexamine/HCl <0°C. The foam filtered off, dried. Yield was just over 50% right on the documented yield.
Melting point on rapid heating was 110°C, close enough to documented temp of 106-7°C. The other possible product (dinitrosopentamethylenetetramine)
melts at 207°C so easy to tell apart.
By not mixing the up the nitrous acid first, theres a lot more foaming and heating and often I end up with nothing at all.
R-salt burns easily with soft orange flame leaving residue, with noise but not as vigourously as RDX. Ive never tried to detonate it.
<center><img src="http://www.sciencemadness.org/scipics/axt/rsalts.jpg"></center>
^ I dont think all of the pics above are from the same batch.
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Rosco Bodine
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R-salt / RDX eutectic
R-salt forms a relatively low melting eutectic at about a 50/50 mix with RDX which results in a very high energy composition . PATR mentions a minor
proportion of a third material used in the composition . Possibly the ethylene or propylene pseudo-nitrosite could also be useful in such a meltable
composition .
With regards to use of N2O3 for R-Salt ,
some means of pH control might give better yields . For example , dissolving
hexamine in white vinegar ( 4 or 5% acetic acid ) in excess and then adjusting
the pH if necessary with HCl , chilling very cold and nitrosating , could give better yields than using HCl alone as the acid as when sodium nitrite
is used as the nitrosation reagent . When the solid nitrite is used it would tend to buffer the reaction pH by virtue of the sodium it contains .
But the use of N2O3 would
be absent that buffering effect which
would cause the reaction mixture to become more and more acidic as the nitrosation proceeds . The effect would be lessened in a reaction mixture
which
is mainly acidified with acetic acid and where HCl is present in lower amount .
There is also the possibility that this approach would not work at all , especially if the acetic acid itself should be nitrosated , or if the
dilution is too great for the reaction mixture of this sort to react as wished .
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Axt
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I'm attaching the article referenced in PATR 2700, which gives the desired pH, takes a ratio of 6M HCl to 1M hexamine to give the trinitroso product.
It mentions that the use of acetic acid alone will produce the dinitroso product, then it shows a less then convenient route from this to HMX.
| Quote: | Originally posted by SAM4CH
Can I convert R-salt to RDX?! more details! |
It is mentioned in PATR 2700 that r-salt can be nitrated to RDX with H2SO4/AN in >90% yield. If N2O3 drawn off H2SO4/AN/starch was to work it could
be a convenient way to RDX, requiring no nitric acid or nitrites. Note that 50% R-salt yield is based on 1M hexamine creating 1M R-salt, with RDX
theoretically 2M are created for every 1M hexamine in ammonium salt is used. This means, through this route, at best you can expect a 25% yield of RDX
from hexamine.
[Edited on 9-12-2005 by Axt]
Attachment: nitrosation of hexamine.pdf (395kB)
This file has been downloaded 3424 times
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Rosco Bodine
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From the information in the Bachmann & Deno article it appears that use of acetic acid takes the pH too far in the wrong direction for R-salt and
leads instead to the DPT material which is primarily useful as a precursor for HMX . The DPT is obtained in better yield more cheaply by simply using
less HCl to raise the pH of the
reaction mixture , so acetic acid offers no advantage .
PATR states that a mixture of R-salt and NG kept at 90C for 5 days showed no apparent decomposition ? Possibly a misprint , because that would seem
to indicate stabilizing properties for R-salt towards nitroesters which if true is very interesting . If this is general , R-salt could possibly have
value as an energetic stabilizer as well as filler for ETN melt and other low melting compositions , and possible usefulness in many other nitroester
containing compositions .
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Rosco Bodine
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Urbanski describes 84% yields of R-salt reported by Aubertein giving detailed instructions for synthesis
P. Aubertein , Mem. Poudres 33 , 227 ,
( 1951 )
Also in the same journal a method for production on a semi-commercial scale is reported by Ficheroulle and Kovache
H. Ficheroulle and A. Kovache , Mem. Poudres 33 , 241 , ( 1951 )
These would be interesting references if anyone has access and may share these articles .
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halogen
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You bubbled N2O3 through hexamine/hydrochloric acid? Why would you need HCl? Just to keep PH down? Why the -NO replace Cl. Is nitrous acid stronger?
F. de Lalande and M. Prud'homme showed that a mixture of boric oxide and sodium chloride is decomposed in a stream of dry air or oxygen at a red heat
with the evolution of chlorine.
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Axt
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| Quote: | Originally posted by halogen
You bubbled N2O3 through hexamine/hydrochloric acid? Why would you need HCl? |
In aqueous solution:
N<sub>2</sub>O<sub>3</sub> + HCl → NOCl + HNO<sub>2</sub>
NOCl + H<sub>2</sub>O → HNO<sub>2</sub> + HCl
And acid conditions are needed to form R-salt opposed to the dinitroso derivative.
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halogen
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I N2O3 was nitrous anhydride. If not, what is?
F. de Lalande and M. Prud'homme showed that a mixture of boric oxide and sodium chloride is decomposed in a stream of dry air or oxygen at a red heat
with the evolution of chlorine.
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