Sciencemadness Discussion Board - HMTD problem

HMTD problem

Melmoth - 15-7-2002 at 09:52

Hello, I'm a new member to this forum although I'm reading it for a longer time now. I finally acquired all the chemicals for HMTD manufacture, but here is my personal problem. I tried to make HMTD yesterday, but after more than 24 hours there are still no crystals formed in the reaction vessel. Here is my procedure;
I dissolved my Esbit tablets in distilled water and filtered off the wax binder, I boiled off the excess water and dried the white crystals.
I mixed 100ml of 10%H2O2 with approx. 10gr of Hexamine. And added 50ml of 32%HCL, the temperature rose to about 30 degrees Celsius (I mixed all the chems in a ice-bad). I left the solution in the fridge and stirred occasionally. Now after more than 24 hours no crystals have formed, what is the problem: did I use too little quantities or is the temperature too low? (There are also many little bubbles on the inside of my plastic reaction vessel)

Try something other than HCl...

Polverone - 15-7-2002 at 14:35

I have had acceptable results using both citric acid and glacial acetic acid. I would try using one of these acids in place of the HCl. I know, there are people who say HMTD can be made with HCl, and they may be right. But I think there's a reason that the standard preps don't use strong mineral acids.

Also, you seem to be using a *lot* of HCl for such a small batch. Did you get these proportions from somewhere or were you just guessing? I would also say that you would be better off using more highly concentrated H2O2, although that may not be possible in your situation. With weaker peroxide you will probably experience lower yields and much longer reaction times, but that's just a guess.

HMTD isn't super-tricky to make, but it's certainly pickier than (say) acetone peroxide. If your reactants are too low of a concentration, or the vessel gets too warm, or stays too cold, you may get nothing at all.

raistlin - 15-7-2002 at 15:20

What is HMTD?

Raistlin

Rhadon - 15-7-2002 at 19:15

I used HCl to make HMTD, with satisfying results. I don't remember exactly how much HCl I used, but like Polverone said: 50 ml should be too much. I think I used something like 10 - 15 ml on 10 g of hexamine. Though, I used 30% H2O2.

Surprisingly I didn't experience such a strong rise in temperature (I don't know from which temperature you were starting. I assume about 15° C) . In fact, I didn't notice a considerable change in temperature at all, and I didn't apply strong cooling (just an ordinary ice-bath, no continued cooling in the fridge).

HMTD stands for hexamethylene triperoxide diamine. Since it is a peroxide it is somewhat related to acetone peroxide (which I assume you already know), and it is said to be less unstable. But I'm sure there are other people who can describe HMTD much better than I can

raistlin - 16-7-2002 at 06:17

Lol, that was a perfect description of HMTD, because I doubt that I would understand if you had got any more complicated...

Raistlin

Melmoth - 16-7-2002 at 09:33

There still aren’t any crystal formed, I left it out off the fridge now for approx 20 hours. I converted my quantities from Mr. Cools site http://www.flashbangboom.homestead.com/home_page.html It was a Saturday morning so the calculations will probably be wrong (I don’t know how I calculated 50ml HCL, but anyway)

I finally got a supplier that sells me 30%H2O2 and I placed an order last week so that should be delivered next week, but since I’m going to Spain Monday, there will be now experimenting for about tree weeks.

HMTD

00Buckshot - 18-7-2002 at 20:10

This morning I thought I'd whip up some fast HMTD, and HMTD isn't wasy to make fast.
I used Hcl instead of my normal citric because I didn't feel like stirring alot.

Anyways I add the Hcl way to fast and it boiled out of control, with plenty of toxic fumes. I had to dump. The citric acid seems better to me, and less toxic.

Melmoth - 21-7-2002 at 04:34

I ordered 30% H2O2 and it was delivered yesterday, but because I wasn’t home they left it at the post office

. Since I’m going on vacation tomorrow I cant pick it up until next week or so. I have done some new calculations with the new chems, but can you give me some ratios? I now have 30%H2O2, 32%HCL (Spirits of Salt) and Hexamine from Esbit tablets.

Melmoth - 3-8-2002 at 00:45

Today I dreamt my new HMTD experiment. I dissolved 7 Esbit tablets into boiling distilled water; I filtered the wax binder off and boiled the excess water off. I dried the Hexamine crystals for more than 24 hours.
I cooled 40ml of 30%H2O2 and mixed it with the hexamine (the reaction vessel already placed into an ice-bad). I measured out 70ml of 32%HCl and poured in 5ml at a time. First the solution was slightly salmon coloured, after approx. 10ml of HCl the solution turned plain again and after 35ml it turned salmon again. After another 5ml, crystals started to form rapidly and I stopped HCl addition. Since all my ice was melted at this time, I put the reaction vessel plus ice-bad into the refrigerator (after each addition the temp raised rapidly).
After my solution has cooled a bit I will add the other 30ml of HCl and let it stand for a while.

Melmoth - 3-8-2002 at 00:47

After an hour a thick layer of HMTD crystals was floating on top of the solution, there were also crystals floating around at the bottom. I dried some crystals that stuck on my thermometer; they ignited with a very rapid and impressive flame. I poured the other 30ml of HCl into the solution (in portions of 5ml at a time). But after another hour al my crystals disappeared! Now, two hours later, I only have a clear solution left. I shall wait another 12-24 hours before my final conclusion, but it seems to me that there was too much acid, it seems that 40ml should have been enough.

HMTD with HCl

Melmoth - 6-8-2002 at 15:23

Maybe an old story here, but this process uses HCl instead of the more commonly used citric acid.

HMTD Manufacture

Materials needed:

40ml of 30% H2O2

30ml of 32% HCl

7 small Esbit tablets

10gm Sodium Bicarbonate

Distilled water

Note: I found the H2O2 at an online pharmacy. My HCl is Hiltons “Spirits of Salt” drain opener. I found two kinds of Esbit packages, one with 20 small tablets and one with 6 big tablets (see pictures) Sodium Bicarb is found at a pharmacy for stomach problems.

Dissolve 7 small Esbit (or 3 big tablets, sold as a box of 6) tablets into distilled water. Filter off the wax binder and boil off excess water. Let the hexamine dry for 24 hours, until you have a fine white powder.

Place the 40ml of 30%H2O2 into your reaction vessel, and Cool in the refrigerator. Than dissolve the hexamine into it.

Place the reaction vessel into an ice bad, and pour in the 30ml of 32% HCl (5ml at a time, because after each addition the temperature rises. 30ml should be enough after 25ml crystals start to form, pour in the other 5ml for sure. After the addition of the HCl crystals start to form, let it stand for 30-60 minutes.

Filter off the crystals and wash under tap water several times. Dissolve 10gm of Sodium Bicarbonate into 200ml of distilled water and mix it with the crystals, stir for about three minutes. Filter off the crystals again and let it dry for 24 hours.

Reaction:

C6H12N4 + 3H2O2 à C6H12N2O6 + 2NH3

Sources:

- Chemical structure, properties and analysis calculated by ChemDraw Ultra, CambridgeSoft Corporation.

- Explosivstoffe, Rudolf Meyer, 5. überarbeitete und erweiterte Auflage, Verlag Chemie, 1979, Basel. Page 146-147

- The Chemistry and Powder of Explosives, Tenney L. Davis. Page 451-453

(Will post pictures soon)

PHILOU Zrealone - 8-9-2002 at 13:02

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

Hexamethylenetetramine (HMT), C6H12N4

pyrofrench - 6-10-2002 at 00:30

I have a pack of "esbit" tablet but I'm not sure that this is Hexamethylenetetramine.
I have the same things that in this URL :
http://www.au-vieux-campeur.fr/gp/asp/produit.asp?codprd=224...
please say me if it is, thanx

Nick F - 6-10-2002 at 05:00

Very interesting idea, Philou.
Perhaps the usually low yield of HMTD is partially because some of it is protonated by the excess acid, and therefore goes into solution? Maybe adding dilute NaOH soln would cause more to ppte?

Lucy - 7-10-2002 at 03:27

Can i use KOH too ?

Rhadon - 7-10-2002 at 06:02

Yes, KOH and NaOH can replace each other in most cases. But remember that the idea of precipitating the HMTD by making the solution alkaline is just a supposition. Give it a try and tell us about the results

TheBear - 26-10-2002 at 09:42

I have been thinking:
When HMTA is disolved in water with an acid to catalyse the reaction it forms ammonia and formaldehyd like this:

C6H12N4 + 6 H2O ----> 6 CH2O + 4 NH3

I might be wrong: but doesn't HCl and CH2O form one of the most cancerogenic materials known to man? This might not be true at all but I read this in "The Library" by swedish infomania. But the text didn't tell the name of this material nor it's chemical formula nor what the reaction looked like.

Flying Dutchman - 30-10-2002 at 14:01

Very intresting,
I'm going to oder some HNO3 so if you would be so kind too think it out in the theory? I will be the test person, thinking of: how much HNO3 compared to Dry HMTD ?
if you would give me the information I would be glad too test it

It's so hard to find reliable material...

Ramiel - 31-10-2002 at 03:14

Most of the sintheses I've read for HMTD are pretty innacurate and lack detail.

on the issue of sensitvity most of them say "very sensitive!!1!!1" or "B1G B00Mzz!!!!!!!1" so i haven't made it, and I dont plan to until i find out more.

Just how sensitive is HMTD?

Flying Dutchman - 31-10-2002 at 04:32

just treat it with alot of respect! treat it like it can detonate every second!
than you would be just fine,
for realiable information I use NBK his synth and I use 15 grams of Hexamine, 50 Gram H2O2 30%(I'll give the volume later.) and 70 Gram HCl 29%)(also the volume later)
I'll post when I have the yield.

andreas - 31-10-2002 at 04:47

I'm wondering what kind of yeilds you guys get when making hmtd.
a few days ago I made up a batch using
120grams H2O2
35 grams hexamine
and 40 grams of citric
I ended up with 33 grams of hmtd wich gave me a calculated yeild of 63% based upon the amount of hexamine. My procedure was: make up an ice bath mix h2o2 with hex cool this to about 0 centigrade than add citric slowly.
My mix didn't reach more than 3 centigrade when adding the acid.
Then let it just sit in the ice bath(quite large). This keeps the temp around 0 centi. for 2 hours, after that the temp slowly rises, and then I leave it there for an aditional 12 hours. After that standard filtering, neutralising and further washing.

Flying Dutchman - 31-10-2002 at 13:48

GRRR! :mad:

my HTMD: 50 grams of 30%H2O2
15 grams of Hexamine
72 grams of 29% HCl
And after 4 and a half hour No Crystal! not even one! GRR :mad:

"
I'll let it stay for 12 hours..
I know I used a lot of Acid.. I'll try too get some citric for now on...
ps. my synth was that from NBK.

madscientist - 31-10-2002 at 14:23

Try neutralizing your solution - it's likely that HMTD will precipitate (not certain though, this is only theory).

MINERAL ACID SUCKS!

KABOOOM(pyrojustforfun) - 31-10-2002 at 15:40

HMTD is my favorite explosive.I have kilos of HMTA and buying strong H₂O₂ in large quantities is easy for me. I make it with megalomania's method (can get citric acid rather cheap). I always got good yields but for the last batch I used mineral acid(HCl and H₃PO₄).with 20 g HMTA & 30 ml H₂O₂(45.5%) I got a thin layer of precipitated HMTD(with citric acid the whole solution was in a form of white thick layer). now it's drying on a filter paper I guess not more than 2 or 3 g!.
I think carboxulic acids are good Catalysts: when a carboxylic acid is used it reacts with H₂O₂ and yields into a per-acid then the per-acid reacts with HMTA to yield HMTD
example:

C₆H₁₂N₄ + CH₂(COOH)C(OH)(COOH)CH₂COOH + 3H₂O₂ =>C₆H₁₂N₄ + CH₂(COOOH)C(OH)(COOOH)CH₂COOOH + 3H₂O => N(CH₂-OO-CH₂)₃N + CH₂(COOH)C(OH)CH₂COOH + 2NH₃

andreas - 1-11-2002 at 08:00

To flying dutchman if you need citric acid you can get it at the farmers supply stores in holland in large buckets of 5kg
I'm willing to send you some I have one of those buckets an this is really a shitload. Contact me at kramrak@hotmail.com I also have msn

Aaron-V2.0 - 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!

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.

.

00Buckshot - 7-11-2002 at 15:25

test

Madog - 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

Happy citric time:-)

Flying Dutchman - 6-1-2003 at 14:41

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

frogfot - 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?

vulture - 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.

Madog - 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

frogfot - 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..

Polverone - 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.

frogfot - 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.

H2SO4

mykhal - 6-4-2003 at 13:30

I had success preparing HMTD from hexamethylenetetramine, 30% or 10% H2O2 and battery sulfuric acid (30% ?) - without cooling ;) .
Well, with cooling, but little bit late.

Citric acid method gave me lower yield.

Cappy - 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]

THE REAL WAY to Make HMTD

XxHMTDxX - 30-9-2005 at 18:34

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

[a bunch of junk was deleted here]

[Edited on 10-2-2005 by Polverone]

Joeychemist - 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.

Axt - 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]

quicksilver - 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.....

Hexamine tablets

MadHatter - 1-10-2005 at 11:11

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.

quicksilver - 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 2402 times

Quince - 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]

Axt - 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, please let this thread die.

Here you can get a suitable tutorial for HMTD

jmasterj - 14-12-2012 at 00:21

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]

detonator - 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.

methode LL

Laboratory of Liptakov - 27-12-2014 at 10:11

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

[Edited on 27-12-2014 by Laboratory of Liptakov]

PHILOU Zrealone - 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]

Laboratory of Liptakov - 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