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megalomania
June 17th, 2003, 04:07 PM
Dhzugasvili
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Posts: 64
From:
Registered: APR 2001
posted 05-22-2001 06:17 PM
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I tried mixing 36% formaldehyde, 200ml with 100ml 25% ammonia water. Left solution to sit, It got hot, but no crystals precipitated and still have not precipitated after weeks its been out there. the recipe said to "let the solution evaporate" If anyone has been able to make hexamine, *PLEASE* tell me how!!


CodeMason
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Posts: 383
From: Your Nightmares
Registered: NOV 2000
posted 05-22-2001 07:03 PM
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1. There are probably impurities in either the ammonia or formaldehyde, when concentrations like that are mixed, it does more than get hot, it make sparks and clouds of smoke! Unless you added them SLOWLY, of course.
2. All the liquid needs to evaporate.


Zero
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Posts: 93
From: ...
Registered: DEC 2000
posted 05-22-2001 09:05 PM
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And shoot me if this sounds stupid, but...
Can't you just buy the stuff? I think Cheaperthandirt.com has it.

~Zero the Inestimable



Agent Blak
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Posts: 766
From: Sk. Canada
Registered: SEP 2000
posted 05-22-2001 09:31 PM
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I salt shaker of tablets is like $5-$7CND doesn't sound very cheap to me. If you have access to a chemical supplier(Fire Fox, Pyrotek.org, etc.) I don't think it is that expensive. but to buy it as fuel tablets itis not cheap.
------------------
A wise man once said:
"...There Will Be No
Stand Off At High Noon
... Shoot'em In The Back
And, Shoot'em In The Dark"

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Jumala
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Posts: 200
From: Germany
Registered: OCT 2000
posted 05-22-2001 10:52 PM
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Here in germany you get hexamine in white cubes under the trade brand "Esbit".
This is also expensive.
But Omikron sells it in plastic bags 500g for 3$.





Mr Cool
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Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 05-23-2001 11:48 AM
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I get about 150g for £3 as fuel tablets, which isn't very expensive. I prefer buying it because it's pure and takes no time or effort.


Dhzugasvili
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Posts: 64
From:
Registered: APR 2001
posted 05-25-2001 09:15 PM
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People, thanx for the info, but I haven't tried obtaining it (probably should according to your replies), and as I wright this response excuse the inaccuracies because i am drunk, but tell me, CODEMASON < HAVE YOU EVER TRIED MAKING THIS SHIT?? If so, what formula did you use?
I have some dirt cheap fuel tablets, they are KOrean, they say, "non-toxic, use for heating toys, etc." tell me, how can I tell if this is hexamine?? I guess It would be toxic if it is hexamine, or am I wrong?



CodeMason
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Posts: 383
From: Your Nightmares
Registered: NOV 2000
posted 05-26-2001 12:20 AM
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Yeah, I made it, I used household ammonia (5%) and Formalin (37% formaldehyde). I used around 25ml formaline and 200ml ammonia, and let it sit in the sun for a while. As the liquid evaporated, the inside of the bowl that was dry had a thin coating of white crystals that looked like salt. Finally, after about 2 days, it had all evaporated. The crystals formed a hard cake on the bottom. I oxidized it and it made HMTD, so I knew it was proper hexamine.


Lem
New Member
Posts: 3
From: Austin, Tx
Registered: MAY 2001
posted 05-26-2001 01:01 AM
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well, check out:
http://rhodium.lycaeum.org/chemistry/eleusis/zwit.menh2.html
it is a paper about making methylamine, but it goes through hexamine to get there. it has some good stuff about possible problems and stuff. (NO kewl spelling [stuph] NBK2000)

megalomania
June 19th, 2003, 11:24 PM
stanfield
Frequent Poster
Posts: 166
From: FRANCE
Registered: MAY 2001
posted 06-11-2001 05:56 AM
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I tried to make hexamine by mixing
100mL ammonia (22%) and 160 mL formaldehyde (30%). The reaction is exothermic (80°C) but no field appears...
Now, I'm trying to boil the olution to evaporate all the water but i don't think it will work....
what's wrong ?

thanx !



Mexican Pizza
New Member
Posts: 23
From:
Registered: MAY 2001
posted 06-11-2001 10:06 AM
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you only have to post it once my friend


John456
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Posts: 105
From:
Registered: MAR 2001
posted 06-11-2001 05:25 PM
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I dunno why everyone says this, i have no problems making hexamine. I use 140mL 40% ammonium hydroxide solution and 280mL 37% methanal (Formaldehyde) in a big 5 gallon tub (because the reaction is so heavy). Usually when i mix them it starts fuming, gets VERY hot and once some sparks even came off it. When this is done and it starts to cool some hex usually settles to the bottom, and the rest forms in about a week of standing in the garage. Boiling will probably destroy the hexamine so i wouldnt try it.
[This message has been edited by nbk2000 (edited June 11, 2001).]



Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-12-2001 04:36 PM
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You know, Stanfield, that I can completly identify with you in this search for how to make this stuff. Check out my post below, but since the last reply i have not attempted to make it again though that last reply is pretty good, go to the site that they recommend, that method might work, I still have to try it though, Will reply again when I do.


stanfield
Frequent Poster
Posts: 166
From: FRANCE
Registered: MAY 2001
posted 06-12-2001 04:56 PM
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"Boiling will probably destroy the hexamine so i wouldnt try it."
Damn, I obtained hexamine (white crystals) but I obtained them by boiling the solution !!! How can I make sure it's really hexamine ?

a_bab
June 20th, 2003, 06:32 AM
Well, since hexamine will hidrolise in hot water there is no way of getting hexamine by the means of boiling the solution.

(CH2)6N4+6H2O--->6HCHO^ + 4NH3^

So the correct recipe is :

In a formaline solution of 40 % add ammonia until the reaction is basic, at a temperature of max. 35 dedrees C .(sidenote: the concentration of the ammonia seems it has no effect). In theory the resulted substance contains 90 % hexamine. The solution should be evaporated UNDER VACUUM at no more than 40 degrees C. The obtained hexamine is dried at 30-35 degrees C. In order to get a pure product, the obtained hexamine is recrystalised from alcohol.

This recipe is a translation taken straight from a russian chemistry book.

FANATICO
January 22nd, 2004, 11:55 PM
Originally posted by a_bab
Well, since hexamine will hidrolise in hot water there is no way of getting hexamine by the means of boiling the solution.

(CH2)6N4+6H2O--->6HCHO^ + 4NH3^

So the correct recipe is :

In a formaline solution of 40 % add ammonia until the reaction is basic, at a temperature of max. 35 dedrees C .(sidenote: the concentration of the ammonia seems it has no effect). In theory the resulted substance contains 90 % hexamine. The solution should be evaporated UNDER VACUUM at no more than 40 degrees C. The obtained hexamine is dried at 30-35 degrees C. In order to get a pure product, the obtained hexamine is recrystalised from alcohol.

This recipe is a translation taken straight from a russian chemistry book.



Hexamine not will denatured by boiling water. this only happen at temperature above 280 Celsius.There's no problem in eliminate water in excess by this method. I get 150 gr of hexamine in this very minute ffrom that way. See at www.chemicalland21.com/arokorhi/industrialchem/ organic/HEXAMETHYLENETETRAMINE.htm

Ropik
April 23rd, 2004, 07:53 AM
I used this methode twice and everytime I got good yield.
This is excerpt from Uncle Fester's Home workshop explosives:


To make hexamethylenetetramine, 2000 grams (1850 ml) of 37%
formaldehyde solution is poured into the enamelled dish. Then to this is
added 1100 grams (1200 ml) of ammonium hydroxide solution. As was mentioned
before, this material is just ammonia dissolved in water, and may be sold
under such monikers as strong ammonia solution 27%, or 58% NH4OH or ammonia
water 26 degree balme. The ammonia solution should either be cooled down in
the freezer before use, or have 250 grams of ice added to it.

The ammonia is added slowly to the formaldehyde with good stirring. A
fair amount of heat is given off in the reaction, and the reek of
formaldehyde and ammonia will get intense for a while until all the ammonia
has been added. Then all the formaldehyde will be tied up, and only a weak
smell of ammonia will remain. Stir some more to be certain that an even
solution has been obtained.

The solution in the pan or dish contains about a pound and a quarter of
product dissolved in a bunch of water. The task now is to obtain the
hexamethylenetetramine, which is a crystalline solid, from the water. To do
this, first the dish is placed on the hotplate, then heat is applied to it
to bring it to a slow boil. As the water boils away, portions of about 15
ml of the ammonia solution are added to it every ten minutes or so. This is
to ensure that enough ammonia is present to keep any formaldehyde which may
be floating around unreacted, tied up.

When about half of the solution is boiled away, the heat should be
removed from the pan and the solution is allowed to cool down to the point
where it is about as hot as hot tap water. Then it is filtered through a
coffee filter placed inside a plastic funnel. This is to remove any gummy
material which may have been formed from the formaldehyde. This gummy stuff
will quickly plug the filter, so be prepared to change the filter several
times.

The liquid which filters through still contains the product. It is
returned to the pan. Its volume should be a little over 2000 ml. It is once
again boiled away until its volume is around 800 ml (1/3 or so of the
previous volume). Now the first crop of product can be obtained. Remove the
pan from the heat and allow it to cool, then cool it further either by
packing the pan in ice or putting it in the freezer. As it cools, a large
mass of crystals will appear.

These crystals are then filtered out by filtering them through the
vacuum filtering apparatus shown in the nitromannite chapter. Feel free to
pack them down a little with a spoon to help squeeze the liquid out of
them. Then the crystals are dumped out onto wax paper. The liquid should go
into a separate jug for temporary storage until all the crystals are
cleaned out of the pan. A rubber spatula will be very handy for scraping
the cling-one off the walls of the pan.

When the first crop has been collected, the liquid is returned to the
pan. Then the crystals of product are rinsed off. To do this, they are
packed back into the filtering funnel, and rinsed off with 190 proof grain
alcohol. A few rinses should remove the smell of ammonia from them. Then
they should be spread out on fresh wax paper until they are dry. They
should have no smell. They should also be clear or white in color.

The liquid which has been returned to the pan still contains a lot of
product. To get it, first pour the liquid into a glass beer pitcher or
similar container. Then about 10 grams of powdered activated charcoal is
added to the liquid. If the lab brand of charcoal called Norite is
available, this is best. Otherwise, the various other types of activated
charcoal will work so long as they are powdered up before use.

This activated charcoal will take up the yellowish color from the
solution. First stir it in for a few minutes. Then set up the vacuum
filtration system again, with double layers of filter paper. Pour the
solution through it. A clear solution should result. If it is still black,
all the charcoal isn't out of it. Wash up the system, change the filters,
and filter some more. If it is still yellowish, add some more activated
charcoal and continue.

The clear solution can now be returned to the original dish, and heat
reapplied to it. The goal here is to evaporate the liquid to dryness and
collect the crystals which are left when the water is gone. Heat it
reasonably strongly at first, then steadily back off on the heat as the
volume of liquid goes down. One does not want to burn the crystals.
Finally, end up with just a warm setting, and drive off the last of the
water. Then scrape out the crystals of product from the pan. The total
yield of hexamethylenetetramine should add up to around 560 grams.

All the hexamethylenetetramine should be spread out onto wax paper
sheets and allowed to dry.


I scaled it a bit down, however.

chochu3
September 28th, 2004, 09:20 AM
Is their any way to substitute paraformaldehyde for the formalin solution