kuykur
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How to make hexamine? Please help!
Those fuel tabs which are talked about are simple nonexistant where I am. So I face myself with the challenge of making my own hexamine from scratch.
The H4ClN + Formaldehyde didn't work. Is there any other way which requires no lab glass and no vacuum source?
Thanks!
[Edited on 13-1-2005 by kuykur]
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chemoleo
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Mix formaldehyde and ammonia, and boil to dryness, don't use flame as the hexamine will ignite once dry and hot (personal experience). Try to
have an excess (stoichiometric) of NH3 so you won't have to deal with more toxic formaldehyde evaporating.
Hexamine is most easily made - I am surprised there is no thread on its making.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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kuykur
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Thanks Chemoleo!
I never heard of this way. Can you give me a little more info?
Any formaldehyde will do? I can get 35 VOL form. I don't know if VOL = % . It seems to have some p-form on the bottom. Will it work?
About the ammonia, does it has to be a solution? what % of NH3? can I use the amm.hcl I got spare making a solution in water?
Oh! And how much would the stochiometric excess should be?
Hope you have some time to answer 
I'm planing to do a detailed write-up about it, both successes and failures. As you very well pointed, there seems to be no data about this.
Thanks.
KK
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chemoleo
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It's very simple, I wouldn't even bother calculating it.
Just take, i.e. 200 ml of 36% formaldehyde, and add i.e. a 10% solution of ammonia (or 25%, or whatever) and mix. While stirring, add ammonia, until
the the solution after mixing smells of it (it heats up too from what I remember, let it cool if it becomes too hot). This means you have achieved an
excess of ammonia, whch is what you want. No, you can only use free ammonia. (Or make a solution of ammonium chloride and add a stoichiometric amount
of NaOH, which liberates NH3 in solution. This you add to your formaldehyde.)
Then let it stand for a day, and boil this down, the NH3 will evaporate, plus the water. Eventually you will get crystals, and dry more until
completely dry. There you have your hexamine.
Other names for hexamine are urotropine, and hexamethylen tetramine. There are some threads on this, and what it is used for. Plus
this gives some info on stoichiometry. The info is all there!
Anyway, this is not one of those experiments where you need to be accurate. Nice and simple.
Oh, and would you like to tell me what H4ClN is? 
[Edited on 13-1-2005 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Joeychemist
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The other names for hexamine;
1,3,5,7-tetraazatricyclo[3.3.1.13,7]decane; aceto hmt; Aminoform; Ammoform; ammonioformaldehyde; Cystamin; Cystogen; formamine; Formin; HEXA;
Hexaform; hexamethylenamine; hexamethyleneamine; hexamethylenetetraamine; hexamethylene tetramine; hexamethylene triamine; hexilmethylenamine; Hiprex;
HMT; HMTA; Mandelamine; methamin; metheneamine; resotropin; 1,3,5,7-tetraazaadamantane; tetraazatricyclo[3.3.1.1(3,7)]decane; UREX; Uritone; Uroqid
and methenamine.
Chemoleo, H4ClN is ammonium chloride, I know , but I have seen it writen this way
before, I'm not sure why but....
[Edited on 13-1-2005 by Joeychemist]
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Thomas Winwood
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Chemical nomenclature normally dictates writing an ionic compound as the sum of its ions i.e. NH4(+) and Cl(-) makes NH4Cl. Same for NaCl, Na3Fe(CN)6
and CsCl. Writing H4ClN implies that the nitrogen is bonded to the chlorine, whereas it's actually in the centre of the tetrahedral ammonium ion.
I\'ve been told having a sig is banned, despite the facility being available. Um...contradiction?
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HNO3
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He's probably using the Hill system, where the elements in the compound are arranged in alphabetical order:rolleyes:. It's dumb.
\"In the beginning, God...\" Wait a minute, God doesn\'t exist!!!!!!!!!! \"OK, in the beginning, ummm, hydrogen...\" Wait a minute, what about the
laws of thermodynamics? \"OK, in the beginning, ummm.....UMMMMM, what\'s left to choose from?
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Chris The Great
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Yeah, it's easy, though I ran out of gas when boiling it down, and was using shitty reagants (blue dyed etc).
Be careful about adding too much ammonia, I did that and kinda tear gasses myself when boiling it 
I didn't wait for a day though, I figured that reaction would finish as I heated it (I was lazy, etc).
Here's a synthesis I found on it a while ago http://basti.borec.cz/_english/e_hmta.html
Would the reaction also work by dissolving paraformaldehyde in ammonia solution?
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Joeychemist
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Yeah Chris, Paraformaldehyde works in the same way pretty much, there is a page on frogfot’s site for making both formaldehyde and hexamine. Look
here http://www.frogfot.com/synthesis/formaldehyde.html and here http://www.frogfot.com/synthesis/hexamine.html and if you even need to make the HN3 look here http://www.frogfot.com/synthesis/ammonia.html
Also her is the thread how to identify hexamine http://www.sciencemadness.org/talk/viewthread.php?tid=3166
[Edited on 14-1-2005 by Joeychemist]
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Chris The Great
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Those pages are great! The fromaldehyde synthesis especially, as formaldehyde is expensive to get OTC, but methanol is really cheap, as well as pure.
The formaldehyde I've bought was 25%, with 7.5% methanol and a huge amount of impurities such as dyes. The methanol I've bought cost the
same amount for 4 times the volume, and is 99.9% pure. Apparently paraformaldehyde bought OTC contains similar impurities.
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Cloner
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How did it fare to make paraformaldehyde? I believed it outside the scope of the basement chemist.
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Pyroz
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Plastic supply store should carry 99% paraformaldhyde for fibre glass resin glue sealer --- its not that expensive to buy and fairly easy to find if
you know where to look for it.
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Joeychemist
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formaldehyde can be found at Wal-mart in the form of a variety of products called Campa Chem for use in recreational vehicle sewage treatment (in the
automotive section). There is one brand that is solid granules, get that, not the solution. The actual chemical is paraformaldehyde, the polymerized
form of formaldehyde, but formaldehyde can also be obtained from this too.
The paraformaldehyde is dyed with an unknown blue dye.The dye can be removed with several small portians of alcohol.Simply wash in ethyl or methyl
alcohol then filter or decant.
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JohnWW
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Paraformaldehyde, a polyether, has the following brief properties:
CAS NO. 30525-89-4
FORMULA HO(CH2O)nH (n = 6 - 100 )
MOL WT. (30.03)n
TOXICITY Oral rat LD50: 800 mg/kg
PHYSICAL STATE White solid, formaldehyde-like odor
MELTING POINT 80 - 155 C (85%), 120 - 175 C (91%), 175 C (95%)
BOILING POINT Slowly sublimes
SPECIFIC GRAVITY 1.25 - 1.35 (86%), 1.30 - 1.4- (91%), 1.35 - 1.45 (95%)
SOLUBILITY IN WATER soluble in hot water (insoluble in alcohol, ether)
pH neutral to litmus
AUTOIGNITION 300 C
FLASH POINT 63 ( 86%) - 93 C (95%)
STABILITY Stable under ordinary conditions (Slowly sublimes to formaldehyde)
GENERAL DESCRIPTION & APPLICATION
Paraformaldehyde is a white crystalline solid formed by polymerization of methanal gas (formaldehyde, HCHO) by heating. It is soluble alkali but
insoluble in alcohol, ether, and water. It is used
as fumigant, disinfectant, and fungicide. It is used to make various resins with mainly phenol (melamine resin; phenol resin; vinylon; polyacetal
resin; terephthalic acid; diphenyl methane diisocyanate, acrylic acid esters).
See http://www.chemicalland21.com/arokorhi/industrialchem/organi... , http://www.epa.gov/pesticides/factsheets/chemicals/paraforma... , http://www.proscitech.com.au/catalogue/msds/c007.pdf
Because it is a polyether, it may be possible to use it to chelate metal cations, including alkali and alkaline earth cations, in organic solvents,
similarly to crown ethers (which are much more expensive).
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