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Aaron-V2.0
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[*] posted on 1-11-2002 at 19:49


I tried the HMTD synthesis last weekend three seperate times and they resulted in nothing! :mad: I used Mega's method to the word (Only I substituted 10X 3% H2O2 for 30%)

500ml 3% H2O2
14 grams Hexamine (First two used Esbit tablets, last I used Colhams tablets.)
21 grams Citric Acid

First batch I mixed the crushed Esbit tablets into the H2O2 and the wax was left on top (No harm to the synth I've heard.) and lowered the temperature to 10C. I then started mixing in the citric acid (Particle size is similar to tablesalt.) and the temperature started... DROPPING! :o

I kept stirring it and after about half an hour and putting all 21 grams of citric acid into the mix it had reached a temp of about 3.9C.

I was pissed so I dumped it.

The second attempt was more or less just to check if it was my chemicals. I had plenty of supplies to waste so I put in the exact same amount of chems into a capped bottle and shook it up for a minute, with no temp rise at all!

So, the next day I went into a lovely camping/hunting store and I see a small package of Colhams tablets that're labled "Hexamine fuel tablets". The interesting thing is that the Esbit brand of hexamine is 14 grams to one tablet (Something like 1"x.5"x.75") and the Colhams are round disks measuring 1" across and .5" tall, they weigh 14 grams to 3.5 tablets! Very bulky for "pure" hexamine" and it had no wax binder at all.

And I mix it all together like the first time, with no temp rises except a brief 3C rise and that's it. I leave it overnight for 12 hours and it's still just a milky H2O2 mix. I looked at the bottle of Hydrogen Peroxide and it says "Stabilized Hydrogen Peroxide." Could that be it? Stabilized?

I'll go find some 30% and try it then, hopefully it's just my H2O2.
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00Buckshot
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[*] posted on 7-11-2002 at 15:25
.


test
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Madog
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[*] posted on 3-12-2002 at 18:57


i got some acetic acid, and now i made HMTD, i used 5g of hexamine and got only 2.3g of HMTD, but i have been haveing fun, it is probaly cause i used 12% H2O2, i will use a better concentration next time



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Flying Dutchman
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cool.gif posted on 6-1-2003 at 14:41
Happy citric time:-)


Well finally got some good citric acid, I'll try Mega's synth in 3 days, Will post results with pics on my site.
I'll post the url when it's done;)
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[*] posted on 10-1-2003 at 12:28


Aaron, since you used 10x times diluted H2O2 you should use 10x times more catalyst, though that would be a totall waste of citric acid. One could probably reuse it..

And again, because H2O2 is diluted and there are alot of water, temp shouldnt rise noticeably. Let it react at room temp next time for 12h or more.

Also, do anyone know if one could use 24% acetic acid for synthesis? How will that affect the yeld?
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vulture
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[*] posted on 10-1-2003 at 16:51


24% of acetic acid should do it. It's just the effect of a low H+ concentration that you need. Although acetic acid is a much weaker acid than citric acid.



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Madog
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[*] posted on 11-1-2003 at 05:15


hmm, read the thread on "new HMTD at theforum" you can actualy find it by searching for "HMTD via scetic acid" on google. in there they mention something about low concentration acetic acid causeing heat. you should cool it if you are to do that. in the normal GAA route you dont have to cool it



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frogfot
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[*] posted on 11-1-2003 at 15:07


Recently i read HMTD synthesis in sciencemadness library, it was taken from Chem Soc journal so it have to be a serious document. But i have a question:
Why do we have to stirr reaction solution for 3 hours at 0*C?

Is it because we want to dissolve citric acid?
Is it because some "strange" reaction goes while its at 0*C, which will increase yeld?
Or will those 3h prevent a runaway when we take out reaction solution in room temp?

Sorry that i ask many questions..
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[*] posted on 11-1-2003 at 18:22


In my experience, the stirring is not important as long as you got everything to dissolve. But keeping the materials cold is important - not because of a runaway reaction otherwise, but because the solution seemed to form a lot of bubbles and hardly any HMTD when it was allowed to react at room temperature from the beginning. I am not sure why this is, but I have had no luck unless I cool the reactants as the instructions say to.
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frogfot
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[*] posted on 12-1-2003 at 06:09


Cool, now things start to make some sence. Now i just thoat that this time at 0*C is needed to convert all HMTA to something.. Before actual conversion to HMTD begins.
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mykhal
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[*] posted on 6-4-2003 at 13:30
H2SO4


I had success preparing HMTD from hexamethylenetetramine, 30% or 10% H<sub>2</sub>O<sub>2</sub> and battery sulfuric acid&nbsp;(30% ?) - without cooling ;) .
Well, <b>with</b> cooling, but little bit late.

Citric acid method gave me lower yield.
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Cappy
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[*] posted on 6-4-2003 at 16:39


Apparently your Espit tablets do not contain hexamine.

Found this at http://www.footprintpress.com/Articles/esbittabs.htm

"What we discovered was the “Esbit alternative.” Esbitk is the brand name of a solid fuel cube. It’s similar to, but burns cleaner than, the old Army fuel tabs made of Trioxane and Hexamine. "

Does anyone what Esbit tablets are made of? What brands besides Colhams are hexamine?

[Edited on 4/7/2003 by Cappy]
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XxHMTDxX
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[*] posted on 30-9-2005 at 18:34
THE REAL WAY to Make HMTD


Ok, here is the real way to make HMTD!!

[a bunch of junk was deleted here]

[Edited on 10-2-2005 by Polverone]
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Joeychemist
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[*] posted on 1-10-2005 at 01:45


Your grammar is atrocious to say the least. I will not begin to point out all that is wrong with your post, but your grammar and presentation will need to be worked on. Second, this is a chemistry and science centered type of forum, not a K3wl explosives site, when posting here please make your posts neat, informative, descriptive, but most of all, make your posts useful. ;)

Also, using teaspoons for measuring amounts of reactants is not a universally accepted method of measurement; maybe you should buy yourself a scale.
:P
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[*] posted on 1-10-2005 at 02:20


I won't be nearly so kind. How about someone delete back past that lame misinformative crap "XxHMTDxX" has posted, thus sending this thread back to 4/03 where it belongs.

BTW, that syth is a kewlified copy of that found in "kitchen improvised blasting caps".

[Edited on 1-10-2005 by Axt]
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quicksilver
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[*] posted on 1-10-2005 at 06:55


Quote:
Originally posted by Cappy
Apparently your Espit tablets do not contain hexamine.

Found this at http://www.footprintpress.com/Articles/esbittabs.htm

"What we discovered was the “Esbit alternative.” Esbitk is the brand name of a solid fuel cube. It’s similar to, but burns cleaner than, the old Army fuel tabs made of Trioxane and Hexamine. "

Does anyone what Esbit tablets are made of? What brands besides Colhams are hexamine?

[Edited on 4/7/2003 by Cappy]


It's possibly Trioxane .... the company simply subsituted for that production run or whatever. This compnay ALWAYS uses hexamine for their suff:
"HEXAMINE FUEL TABLETS"
TOCR SPORTS
2732 W. COLORADO AVE.
COLORADO SPRINGS, CO 80904
VERY inexpensive, will ship anywhere, and has no binder, wax, etc. Was actual surplus material. Available is bulk carton or case (1lb - 24lbs) or individual 250gram packages.


But more importantly you raise a point that many chems are being taken off the market or subsituted if enough notariety is directed toward them (note "Red-Devil" lye)
Appolgies if this last sentence is OT.....




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[*] posted on 1-10-2005 at 11:11
Hexamine tablets


I use old military surplus hexamine fuel tablets. They're labeled:

"FUEL, RATION HEATING (INDIVIDUAL)
HEXAMINE"

Bought a 9 LB case of the suckers on eBay a few years ago. I've never had a
problem making HMTD or RDX with them.

If Trioxane is the problem, look around for the military stuff.




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[*] posted on 2-10-2005 at 09:17


Quote:
Originally posted by Axt
I won't be nearly so kind. How about someone delete back past that lame misinformative crap "XxHMTDxX" has posted, thus sending this thread back to 4/03 where it belongs.

BTW, that syth is a kewlified copy of that found in "kitchen improvised blasting caps".

[Edited on 1-10-2005 by Axt]



That type of post is very dangerous and certainly does not belong in a forum discussion on energetic materials. What in God's name is a teaspoon or "cold" or a contrivance of kitchen-measurments doing in a discussion of this material. Peroxides have enough danger without this issue of non-science. -=Very bad stuff=-
Sometime back there exists a study of energetic peroxcides wherein the participants isolated the potential pitfalls in decompensation (w/ TAPT). It was entitled "Decomposition of a Multi-Peroxidic Compound: Triacetone Triperoxide (TATP)" and therein gave some very important information re: longevity, safer mfg issues, etc.
That would be an interesting postulate to this discussion on HMTD....but the KeWL BaUmB-Kid$ stuff is very off-putting.

The references in the article are most important: some discussion centered on this issue on E&W and the references are of value for anyone working w/ this compound. It's just text so you can cut/paste to suite your needs..it's rather lengthy.

Attachment: TATP-article.txt (27kB)
This file has been downloaded 2165 times





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[*] posted on 8-10-2005 at 04:37


Quote:
Originally posted by raistlin
What is HMTD?

Raistlin

LOL! And I get yelled at for not using search here or on the web...

Goto: Google
Type: HMTD
GotoFirstResult: (hit 'I'm Feeling Lucky' button)
FirstSentence: "Does anyone know the specs. on how to use Hexamethelenediammine peroxide (HMTD) as an initiator ?"

Also, it's a very crappy explosive. Doesn't last worth shit. Expect failed detonations if using old HMTD (that's not to say it's safe to handle if old; keep wetted by alcohol -- safer, and unlike water dries fast when need arises to use it).

[Edited on 8-10-2005 by Quince]




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Axt
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[*] posted on 8-10-2005 at 05:06


Quote:
Originally posted by Quince
LOL! And I get yelled at for not using search here or on the web...

And now again for REPLYING TO A THREE YEAR OLD POST! saying "search google". Unless theres actually something new to add to this discussion, <i>please</i> let this thread die.
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[*] posted on 14-12-2012 at 00:21
Here you can get a suitable tutorial for HMTD


This App provides all info needed for making HMTD. With a list of chemicals and production hints.

GOOGLE PLAY - HMTD APP

Greets

[Edited on 14-12-2012 by jmasterj]
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[*] posted on 22-12-2012 at 23:24


Mixed 30ML hydrogen peroxide and 10ML phosphoric acid, temperature, the beaker into the water until the temperature close to room temperature, slowly add methenamine at this time, the solution temperature rises rapidly, when added Urotropine to the beaker scale line 48ml about (10.64g Urotropine), the bottom of the beaker, a white precipitate appeared, the temperature continues to rise, there is a small amount of bubbles. Handheld beaker in the pot in a circular motion, the purpose is to let the the beaker walls of rapid and uniform cooling. When the temperature of the solution is greater than 60, methenamine will be dissolved oxygen does not produce HMTD obtained when the temperature is below 60 degrees, and the product remains substantially constant rate of 70% -75%. 2 ~ 5 minutes solution after the upper has been cropped many of the foam, the temperature dropped to five minutes appears at the bottom of the large amount of surface powdery precipitate after 10 to 20 minutes, there is no longer any phenomenon continues (except bubbling), precipitation is no longer increase. After washing, quantitative filter paper filter to give HMTD finished, the process is only 30 to 50 minutes.
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Laboratory of Liptakov
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[*] posted on 27-12-2014 at 10:11
methode LL


Here I would like to bring my experience. Rule No.1)
The temperature of all components not exceed + 3C. The first 3 hours. Best is 0C. Especially when mixing H2O2 + methenamine not exceed. The procedure is as follows: Refrigerate 45 g of 30% H2O2 at -10C. Dry HMTA powder 14 g cooled on the -10C. Thereafter 14 grams HMTA to 45 grams H2O2. In one step. Closed glass, hand-shaken about 2 minutes. Absolutely clean glass without the presence of metal. (cap). Glass into ice and water. Stir 1 minute in cool water+ ice. Again manually shake for 2 minutes. Shortly, until complete dissolution HMTA. Take 7 grams citric acid crystals and dissolved in one step. Shaken 2 minutes until dissolved. At this stage there is no fear of spontaneous increase in temperature. Conversely. When dissolving acid, will be spontaneous cooling. Again added 7 g acid. Shaking to dissolve. The same is repeated once more. Thus, a total of 21 grams acid to dissolve. Glass into the water and ice. Time 3 hours. Temp. 0C. Without stir. After 3hrs: reheat slowly (15min) on the 25C. When glass 20C is still a clear solution. However: when the temperature will be near 25C over 1-5 minutes the solution became cloudy. Like milk. This is the first Hexamethylene triperoxide diamine. This moment carefully!
Solution slowly circle and temperature monitoring. The glass themselves slowly heated to 30C. At this stage the glass must to cool on the 20C. (in water 5C). Then again, remove from water and slowly stirred maintain the temperature between 20-25C. Glass may be not hotter than the hand. Every 5 minutes stirred 15 sec. Do it about 1 hour. Every 10 minutes/ 30 sec. Still maintain 22-26C. The solution becomes a slurry. After a two hours a dense slurry. If the slurry is thick, like honey, the temperature does not rise any longer spontaneously.
Or only a little and slowly. A thick slurry formed after 2 hours, this is good result. Maintain at 20C still 4 hours. Or longer. In a water bath 20C of about 500 ml. Thereafter filter, extraction, neutralize. Yield is high, very dense slurry. Precise yield I bring later ...:cool:...LL
EDIT yeld: wet HMTD 34,46g. Appart on the 5 parts 6,89g. 6,89 dryed on the 2,80g. 5x2,8 = clear 14,00g HMTD

hmtd.jpg - 26kB

[Edited on 27-12-2014 by Laboratory of Liptakov]
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PHILOU Zrealone
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[*] posted on 30-12-2014 at 05:52


@Laboratory of Liptakov,
Avoid by all means, to store dry HMTPDA (HMTD)(HexaMethylene-TriPeroxyde-DiAmine) into glass jars or hard recipients...in case of unexpected detonation...hard means shrapnels.

@All readers,
N(CH2-O-O-CH2)3N. 2HC(NO2)3 (HMDT dinitroformiate)
Is also another good candidate.
C6H12N2O6.2HC(NO2)3 = C9H14N8O18 --> 2CO2 +7CO + 7H2O + 4N2
Up to now I stil haven't found info on pKa or pKb of HMTD.

Also another interesting question is that usually tertiary amines do form N oxydes upon treatment with H2O2...
What about HMTD di-N-oxyde? O=N(CH2-O-O-CH2)3N=O

Quote: Originally posted by PHILOU Zrealone  
It is good to see despite there are good working procedures, people are stil trying to go the other way to prove it could work!
Why citric acid is favourised vs HCl?
Simply because hexamethylene tetramine is a base and is neutralised by strong acids; a weak acid like citric will neutralise it aslo but the enrergy involved will be lower so will be the heat.A good thing to test, is to neutralise hexamine with HCl; then to cool down and add H2O2!
I suspect that since HMTD (Hexamethylen diamine triperoxid- N(CH2-O-O-CH2)3N) is a diamine, it will also act as a base; hence adding more HCl will lead to the dissalt of it what should be more soluble and thus harder to isolate/cristallise.

This tread gave me a new insane genious idea (amongst many other):the idea would be to make HMTD, isolate it as fine cristals, wash them and then make them react with dillute ice cold HNO3 or HClO4 to get disalts!Then slowly evaporate the water to get
N(CH2-O-O-CH2)3N.2HNO3 (HMDT dinitrate)
N(CH2-O-O-CH2)3N.2HClO4 (HMDT diperchlorate)

1)C6H12N2O6 --> 6CO + 6H2 + N2
2)C6H12N2O6.2HNO3 = C6H14N4O12 --> 6CO + 6H2O + H2 + 2N2
3)C6H12N2O6.2HClO4 = C6H14N2O14Cl2 --> 4CO + 2CO2 + 6H2O + 2HCl + N2

So on a theorical level and based on my knowledge: power should be higher since density will be higher, oxygen balance is improved (thus energy output is higher); what is uncertain is the stability.

If you ever attempt to do this make it in tiny amount since this hasn't ever be done...so treat those two new compounds as if they were NH3.NI3 cristals with the power of HMX.

If they are stable enough to be isolated, you should expect a boost up on VOD level of +2-3km/s (vs 4,5-5,5 km/s for the HMDT).

PH Z


[Edited on 30-12-2014 by PHILOU Zrealone]




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[*] posted on 30-12-2014 at 11:00



Glasses is from the production process. How thick slurry formed. Unfortunately, I did not write it. Certainly, the resulting product is stored in ethanol in a plastic container. Before filling dried always and only 1 gram HMTD. For filling 3-4 primer. It is interesting that nitro-HMTD and perchlorate HMTD. But: The spreading HMTD in perchloric acid? Well .. hmm ... I will not try...:cool:...LL
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