hexamine manufacturing

[andreas]

I've read somewhere a procedure for making hexamine with ammonia and formaline does anybody know how becouse I couldn't find anything.

[vulture]

It's made by recristallizing a stoichiometric mixture of formaldehyde and concentrated ammonia solution. I'm not going to calculate it for you....
Watch out with formaldehyde, it's very toxic.

If you're from holland check a camping store for esbit solid fuel tablets, much easier.

BTW, all of this has been covered before.

[10fingers]

Yes, you can make hexamine this way and it is fairly easy. You can use either formaldehyde or paraformaldehyde.
The ammonia needs to be of a much higher concentration than you can buy in the store but the store bought stuff can be concentrated easily.
The procedure for doing this is very easy to find if you look. It's in Uncle Festers Home Workshop Explosives, Kitchen Imp. Plastic Explosives and I think in Megalomanias Controversial Chem Lab, and a few dozen other places.

[RTC]

http://80.3.211.11/top.JPG
http://80.3.211.11/side.JPG

Store brought hexamine.

[DBSP]

I'm gona have to start making my own hexamine since the only source of pure hex has run out. Extracting from esbit isn't an option since that would mean a 50$ price per kg. I'll be ordering some chems next week and then I'll order .4 kg paraformaldehyde. I don't remember the ratio though.

[xoo1246]

Where are you buying you paraformaldehyde DBSP?, you didn't respond to my mail.

[rikkitikkitavi]

chemicals:
<a href="http://www.svenskakemi.nu" target="_blank">www.svenskakemi.nu</a>

utensils:
<a href="http://www.makab.se" target="_blank">www.makab.se</a> (expensive, but a lot)
<a href="http://www.sagitta.se" target="_blank">www.sagitta.se</a> (cheap)

take it easy and dont blow of any vital parts, so
that these companies stop selling to "civilians" :)

/rickard

<small>[ March 30, 2002, 07:27 PM: Message edited by: rikkitikkitavi ]</small>

[stanfield]

you said I could make hexamine with paraformaldehyde ?
I'm very interested to know the equation of the reaction with para 'cause I have a bit less than 1 Kg since my attempt to do RDX with E process never worked for me...

a big thanx !

<small>[ March 31, 2002, 03:03 AM: Message edited by: stanfield ]</small>

[xoo1246]

rikkitikkitavi: svenska kemi is closing down their laboratory chemical section.

[DBSP]

Sorry Xoo I've had problems logging into my mail, I just got in.
The paraformaldehyde is in "lagerlistan" at svenskakemi. It's about 0.4kg for 13,9$ (139kr exkl. moms).

The process of making hexamine with para and NH3 is very simple, it's just to mix the ammoniak with the para(aq). I don't remember the ratios but they are in this forum somewhere. I'll try to find them as soon as I can.

[stanfield]

did a search but found nothing about ratio... so, could paraformaldehyde be considered like 100% formol ? if, yes, the equation is the same, only amonts of product will change...

6CH2O + 4NH3 --> (CH2)6N4 + 6H2O

see ya !

[DBSP]

That might be right, as I remember it a 37% formaldehyde solution is used. I haven't quite got this yet, what's the differens between paraformaldehyde and formaldehyde. Does the Para get converted to formaldehyde when added to water?

Look at post number 6. at:http://www.roguesci.org/cgi-bin/ewforum/ultimatebb.cgi?ubb=get_topic;f=3;t=000336

I found the post I was looking for, It was Mr .evil who made his own hex.

hey al,
why do you use esbit fuel tablets?
maybe there's a pollution in it...

but anyway,
i make my hexamine/methenamine myself.
by adding formaldehyde-solution and ammonia together(200/450ml.).

next.
i let it sit for lets say:24 hours.
i heat it and the crystels begin to appear.

the result;
100% pure home-made hexamine.

but i suppose you didn't have acces to formaldehyde-solution.

with kind regards,
Mr.Evil

Mr .evil are you arround here, could you give us any comments?

[Lagen]

I have a procedure for it on my site, but the yield was always crap. I gave up on it, as I'm getting HMTA real cheap at about $3.35/kg. (How much is in that pack of hexamine above there? A pound?)

Anyways, the theoretical ratio is 50ml 37% formaldehyde and 35ml 24% ammonia. In grams that's 20 g paraformaldehyde and 7.64 g ammonia. Paraformaldehyde isn't hydrolised spontaneously to formaldehyde in water (or just very slowly), but that doesn't mean it can't be reacted.

That's an incredible price for paraform. I'm getting that amount of (HCHO)n at $3.31.

[DBSP]

Yes it's very expensive, but that's the only source I know of.
I just checked another company, they sell 5l 37% formaldehyde for about 20$, but they don't sell to privates. <img border="0" title="" alt="[Frown]" src="frown.gif" />

[Lagen]

Even that's expensive, well to me anyways, you could buy 5l over here for about 12$ in the hardware store. I checked a chem supplier that sells to individuals, 5l for $9.50.

[RTC]

I think there's a pound, I never weighed it, Anthony you've used these before, did you weigh them?

[10fingers]

It's usually much easier to buy hexamine than make it. I can get it for $7.00 per 454 gms. The paraformaldehyde alone to make it will cost me that much. But I did try it once out of curiosity. I think using paraformaldehyde is cheaper than formaldehyde. I just used some crappy portable toilet disinfectant and concentrated store bought ammonia and I was surprised at the amount of hexamine I got.
When I did it I was not sure on how much paraformaldehyde to use, the procedure in UFHWE uses 37% formaldehyde. I put like 100 gms of paraformaldehyde in a container with about 1 liter water. I heated it to help the paraformaldehyde to dissolve. I added concentrated ammonia solution a little at a time while stirring with gentle heat. The paraformaldehyde dissolves slowly so theres no point in adding ammonia faster than it can be used in the reaction, it will just evaporate off and be wasted. I just kept adding ammonia until all the parformaldehyde had dissolved.
When the rxn is over you gently heat the solution until it is down to 1/2 it's original volume, let it cool down and filter. Heat it some more until it starts to get syrupy. Place it in fridge to crystallize out. Remove crystals and repeat concentration and crystallization 2 more times. To purify I crystallized again from methanol.

[DBSP]

Off cource it's easier to buy it but the only source of pure hex has run out so I can't buy it anymore. That's why I intend to make it since it would cost very much to extract from esbit. I've never seen formaldehyde here in a store.

[xoo1246]

DBSP: I found a place where you can see what chemicals some paint stores sell. <a href="http://www.inkopsguiden.com" target="_blank">http://www.inkopsguiden.com</a>

[Anthony]

I don't know, I've never weighed a pack, but at least 1/2lb I reckon. I can't remember exactly how much, but I definitely don't pay £2.99 for mine, it's less than that.

[vulture]

If you're really in need of hexamine check pharmacies.
They sell it 99.99% pure but it's expensive. Have an excuse ready, although i doubt much people know you can make explosives from hexamine...

[Mr Cool]

I'm surprised hexamine isn't banned everywhere! It is a precursor for all kinds of drugs and explosives, yet I can still buy it in every camping shop I know of.

A tip to those buying it as fuel tablets: look for an army surplus place, I just found out that they normally have it cheaper (like 50p per pack). A pack contains about 170g.

[DBSP]

I have no problems buying hexamine. The problem is the price, if I were to buy a kilo of hexamine (extracting from esbit) that would cost me over 50$ and that is very expensive. Since I have no idea of the yield when making it myself I can't be shure of the price but I would probably end up cheaper than the esbit.

[mongo blongo]

Just wondering why some people are saying "extracting the HMT from the fuel tabs"? My tabs are pure and can be used straight away. Do yours have any funky stuff in them or something?

[Yi]

My ones have wax to protect them from moisture.

<small>[ April 02, 2002, 10:43 AM: Message edited by: Yi ]</small>

[DBSP]

The esbit tabs weigh 4g and they contain 2,9g hex wich means 1,1g of impurities, wax and stuff.

[mongo blongo]

Ah I see, that must be a pain in the ass! All the brands I have had (about 3 or 4) have just been pure! Just crush em up and go! :)

[S. Toppholzer]

I saw anydrous Paraformaldehyde has been mentioned here - anyone got any raios? I've got a full kilo of Paraformaldehyde at home - 'twas never opened. Since RDX manufacture won't work I guess I'll make my own hexamine with it.

[10fingers]

For the ratios read back up this page to a post by Lagen.

[mr.evil]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">That might be right, as I remember it a 37% formaldehyde solution is used. I haven't quite got this yet, what's the differens between paraformaldehyde and formaldehyde. Does the Para get converted to formaldehyde when added to water?

Look at post number 6. at:http://www.roguesci.org/cgi-bin/ewforum/ultimatebb.cgi?ubb=get_topic;f=3;t=000336

I found the post I was looking for, It was Mr .evil who made his own hex.

hey al,
why do you use esbit fuel tablets?
maybe there's a pollution in it...

but anyway,
i make my hexamine/methenamine myself.
by adding formaldehyde-solution and ammonia together(200/450ml.).

next.
i let it sit for lets say:24 hours.
i heat it and the crystels begin to appear.

the result;
100% pure home-made hexamine.

but i suppose you didn't have acces to formaldehyde-solution.

with kind regards,
Mr.Evil

Mr .evil are you arround here, could you give us any comments?

</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Yes i'm here <img border="0" title="" alt="[Wink]" src="wink.gif" /> , this morning i readed this thread...
i got my Formaldehyde solution from a company called 'brinkman' they are dutch, but have stores all around the world(Belgium, France, UK, Spain, Poland, Hungary, China....) they sell it in bottles of 1L and in jerrycans of 20l, not very expensive, i thought it was around 27$/20l

The NH4OH solution i get from belgium, 25% per 5litres 4$, but common household 5% works wel...

Cya

[S. Toppholzer]

As far as I know Paraformaldehyde powder cannot be diluted in water??

[mr.evil]

hmmm, i have some formaline in my lab, what is a solution in water AND Methanol to stabilize it...

i've just found a new chemical supplier from Holland, they sell Formaldehyde tablets 99% pure, so you can make your solutions your self...

once and again, check the agrarical shops(damn, i love them!) they sell HNO3,Urea,HCl,I2(in water and alcohol),H2O2(35%), Formaline (40%) and many nitrates...(such as MgNO3, KNO3, NaNO3 etc.)

Cya

<small>[ May 02, 2002, 07:39 AM: Message edited by: mr.evil ]</small>

[jarrod]

mongo blongo, what exactly where those brands for the hex tabs? I have been looking around for a while to find pure or close to pure tabs.

thanx

[mongo blongo]

Oh hell I can't remember their names.I remember one of them was made by something "teck" (one word) in a green box with a photo of people camping out on it. I will have a look next time I am in that area. I doubt that you will have the same brands in Australia though.
Only one of the brands actually stated that they were hexamine but you can tell by the smell (they smell like shit) and they smell even worse after they have been burnt. If you find any fuel tabs in a camping shop then they are almost defiantly hexamine. In fact I can't find any that are not hexamine (I was looking for the trioxene ones).

[jarrod]

I went and bought a pack of hexamine tabs, but I’m not sure wether they are pure or not
I’m pretty sure that they some kind of wax binder and wax on the outside for waterproofing.(because i can feel it) Would wax be my only impurity??

If I crushed up the tabs and dissolved in distilled water then “scooped” out the wax on top. Then boiled the remaining liquid until dry powder was left. Would this get rid of my wax impurity?

Are there any other ways of purifying hex tabs?

thanx

[vulture]

Your hexamine should be pure enough for "production" <img border="0" title="" alt="[Wink]" src="wink.gif" /> now.
I don't think there's any better way of getting rid of the wax. Acetone or alcohol will probably dissolve the wax too to some extent, which would make separation impossible.

[ossassin]

A brand called "Coghlan's" makes hexamine tabs that appear to be pure. They are very rough, and don't feel waterproof. I am not sure how to tell if they are pure hexamine. I hope that sort-of answers your question about which brand to use. (These are sold in camping and sporting goods stores all over the US. Mine were $2 for 24 tablets. I haven't weighed them yet.)

[A.Scriabin]

Does anyone tried to make hexamine from formaldehyde and ammonia?My yield is too low!I've mixed the components at 3°C and now(one day later)I evaporate the solution,but the yield is about zero :( !

[knowledgehungry]

If you want help you need to give a step by step account of the procedure you used, and the amounts of reactants you used.

My guess is that you used too low of a concentration of ammonia but with the pitiful lack of information you posted, that's just a shot in the dark.

[A.Scriabin]

I'm sorry,but I made a mistake!When I write my previous post,the solution was almost dry,not totally dry...and it was clear,so I thought that the yield was really bad;However now the solution is entirely evaporate,and there is a lot of white precipitate(with orrible smell).I think this happen because the great solubility of the hexamine.

(sorry about my bad english)

[rayman]

Scriabin, would you please post your method, as well as the ending quantity

I Have been looking at this method for a while

[joeflsts]

This is an expensive way to make Hexamine but it did work:

*Do this outside or in a hood.

Hexamine Synthesis
(Methenamine / Hexamethylenetetramine)

Materials:
50ml 36.5 - 38% Formaldehyde Solution
100ml 10% Ammonium Hydroxide Solution

Placed 50ml Formaldehyde Solution in 250ml vessel in ice bath with magnetic stirrer. Allowed Formaldehyde Solution to sit, with stirring, for approximately 15 minutes to insure temperature drop.

Place 100ml Ammonium Hydroxide Solution in 250ml Seperatory Funnel and slowly added Ammonium Hydroxide Solution to Formaldehyde Solution. This process took about 30 - 45 minutes. I wanted to keep reaction mixture cool and the reaction is highly exothermic.

After all Ammonium Hydroxide Solution was added I placed a rubber stopper on the vessel and placed it in an ice bath for 24 hours.

I evaporated the water to dryness @ 100C. At this point a white participate started to form (Hexamine). I place the participated Hexamine into a crucible and heated in the oven for 1hr @ 166C until anhydrous Hexamine was fused.

Final Yield: 9.3g - This is a guess because I got sloppy.

Burn Test - Burn with no smoke.