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Melmoth
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[*] posted on 15-7-2002 at 09:52
HMTD problem


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)




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[*] posted on 15-7-2002 at 14:35
Try something other than HCl...


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.
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raistlin
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[*] posted on 15-7-2002 at 15:20


What is HMTD?

Raistlin




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[*] posted on 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 :)
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[*] posted on 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




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Melmoth
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[*] posted on 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) :D 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.



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[*] posted on 18-7-2002 at 20:10
HMTD


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.
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[*] posted on 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.
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Melmoth
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[*] posted on 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.




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shocked.gif posted on 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.



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[*] posted on 6-8-2002 at 15:23
HMTD with HCl


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)




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[*] posted on 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
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[*] posted on 6-10-2002 at 00:30
Hexamethylenetetramine (HMT), C6H12N4


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:)
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[*] posted on 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?
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[*] posted on 7-10-2002 at 03:27


Can i use KOH too ?



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[*] posted on 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 :)
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[*] posted on 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.
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[*] posted on 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:D:D
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[*] posted on 31-10-2002 at 03:14
It's so hard to find reliable material...


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?
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[*] posted on 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.
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[*] posted on 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.
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Flying Dutchman
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[*] posted on 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.
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[*] posted on 31-10-2002 at 14:23


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



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[*] posted on 31-10-2002 at 15:40
MINERAL ACID SUCKS!


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
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[*] posted on 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:)
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