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Author: Subject: Can anyone figure out what this may be??
iv81
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[*] posted on 3-10-2006 at 16:12
Can anyone figure out what this may be??


http://www.youtube.com/watch?v=r7gyuR-G6vM :o:P

[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 3-10-2006 at 17:06


Far out .

Welcome to SM .

A guessing game ? Okay let's play .

You said a polymer is involved .

Are one or both precursors organic oxy-acid salts ?
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iv81
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[*] posted on 3-10-2006 at 18:12


Thanks,

To be honest, although I'd love to learn chemistry I don't know much but simple concepts of applying one thing to another.

The two chemicals were used to make this are:

NH4ClO4 and C6H12N4 in ratios of 7:3

Could you possibly describe what might have formed or if there is already a name for this reactive compound.

Neither chemicals have melted when heated separately. So I came to a conclution it may be some form of polymer. Is that the correct term?

[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 3-10-2006 at 19:47


Coincidentally there was discussion here recently about
the possible reaction of trioxane with ammonium perchlorate and the possibility of detonation of the
methylamine perchlorate and dimethylamine and trimethylamine perchlorates which could also form , if
the temperature was too high . It was the Perchlorates compositions thread here in this section .

http://sciencemadness.org/talk/viewthread.php?tid=6334

You really must be very cautious heating this sort of mixture , which I am sure you have your own keen awareness , and what may be relatively safe for a couple of grams may be suicidal in larger amounts by the same method . There is probably a much safer way of reacting
the materials which can be worked out with some experimentation .

Hexamine is what you are using there , usually written as (CH2)6N4 , and upon heating , the hexamine can act as a formaldehyde donor similarly as trioxane , which is three formaldehydes as a cyclic condensate sort of polymer .

Did you get a smell of ammonia coming off the mixture
as it was reacting ?

[Edited on 4-10-2006 by Rosco Bodine]

Attachment: GB168333 methylamine perchlorate.pdf (151kB)
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nitro-genes
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[*] posted on 3-10-2006 at 20:17


C6H12N4? Do you mean hexamethylenetetramine or hexamin? :)

If so, my guess would be that your mixture will consist out of many different compounds that are formed simultaneously under these conditions. If subjected to heat and/or acidic conditions, hexamine decomposes easily, forming mainly ammonia and formaldehyde, though all kinds of methylamines, guanidine, formic acid are produced too. Formaldehyde can react with ammonium perchlorate (AP) to produce methylamine perchlorate. Also, the acidic ammonium ion will be displaced by hexamine upon heating, (did you smell an ammonia odour?) forming mono en diperchlorate salts of hexamine. IIRC these are hydrolized rather easily, forming yet other products. Exssive heating will eventually start randomly oxidizing many of the formed species as the AP start to decompose, producing chlorine, oxygen and water and is likely the cause of the coloration of your mixture towards the end of the heat applied...
I have noticed that ammonium nitrate/hexamine melts also produce yellowing and darkening upon prolonged and strong heating, though not as quickly as with ammonium perchlorate which is more acidic...

Many organic perchlorates are very hygroscopic, so the viscous end product is most likely a sort of high percenatge water containing eutectic/solution of all kind of randomly formed rubbish... :D

Looks cool though! ;)

Did you try somewhat "milder" heating methods than a gasfurnace, to drive off any water?

[Edited on 4-10-2006 by nitro-genes]
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iv81
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[*] posted on 3-10-2006 at 20:33


Thanks you guys, yes it was Hexamethylenetetramine with Ammonium Perchlorate.

The smell as heated was somewhat sweet like faint vanila smell or simmilar. I don't know the hazards to it so I tried to avoid brolonged inhilation.

And n-g, I have gently boiled away the water off the camera on the same heat source.

I am hopping if somone with more knowledge as yourselves could repeat this experient and do more tests on it to determine what else is possible. :P


[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 3-10-2006 at 20:44


The reaction can probably be done in aqueous solution
as a parallel to the patented method for methylamine nitrate , and then the product secured by evaporating the water away .

I think using formaldehyde solution , or formaldehyde
solution freshly made from parformaldehyde or trioxane ,
along with a bit of urea , and the ammonium perchlorate
would react in hot solution similarly as the attached patent describes for the nitrate analogue . The quantity for the
perchlorate must be adjusted for the difference in mole weight .

Attachment: EP0037862 methylamine nitrate.pdf (425kB)
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Rosco Bodine
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[*] posted on 3-10-2006 at 20:59


Ammonium Perchlorate has a mole weight of 117.49
Ammonium Nitrate used in the patent has a mole weight of 80.04 . So for the substitution of perchlorate for nitrate
you should use 117.49 / 80.04 or 1.47 grams of NH4ClO4
instead of each 1 gram of NH4NO3 .

There is another patent attached which better shows some of the reactions . But the other patent which utilizes urea
as an additive is a more advanced method .

[Edited on 4-10-2006 by Rosco Bodine]

Attachment: GB1548827 methylamine nitrate related.pdf (320kB)
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iv81
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[*] posted on 3-10-2006 at 21:09


So it's possible that this stuff is able to be detonated as high explosive would.? :o

[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 3-10-2006 at 21:25


You got it , that's what it is , a high explosive and
a fairly sensitive one .....if it is what I think it probably is .

And if it is , you should know that even that small amount
which you were experimenting with could take off your hand and blow that gas burner through the top of the stove and into the oven below , probably rupturing the gas line and causing secondary problems we won't go into . So it is probably good to not pursue the inevitable ,
but find a better way .

[Edited on 4-10-2006 by Rosco Bodine]
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[*] posted on 3-10-2006 at 21:35


Uhh oh.. ok I'm going to go flush few things down the toilet.. Excuse me! :o
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Rosco Bodine
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[*] posted on 3-10-2006 at 21:44


Don't get freaked out about it just keep your wits
and study the reaction under safer conditions .....
you'll live longer .
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[*] posted on 3-10-2006 at 21:56


Well, ok I've tried burning one gram of this substance all at once before. It just burned up pretty fast with a big flame/whoosh leaving some dark unwashable stain on the pan with some diamond shaped patterns. So at least I'm not that concerned but I'd proapbly agree that it capable of detonating with some cap maybe.



[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 3-10-2006 at 22:08


The methylamine perchlorates are white in color so
whatever are the darker products are probably decreasing the yield and purity . The energetic
components of the mixture are probably at their peak
earlier and you are cooking it too long and too hot .
I am sure I heard a small pop from some of the boiling material spattering onto the burner very early in the
video , so it is likely the reaction you are wanting
is already at completion well before the color change ,
and all you need thereafter is to evaporate any remaining water using a much gentler heat source ....
which would really be good for the entire reaction , as
you don't need nearly so much heat . The reaction should proceed even at the temperature of a slow cooker ......a crock pot on low would be more sensible than a gas burner . Let it react at near the boiling point
for a few hours and then let it bake the water out
at the same very low heating for a few hours more .

I think if I was doing it like the EP0037862 patent ,
that I would add some denatured alcohol to the
mixture during the drying stage , to esterfy the 1% or so
of formic acid byproduct to ethyl formate which would
escape with the water .....and leave a purer product
as well as helping the evaporation of the last of the water
by using some excess of ethanol beyond that needed for the
ethyl formate .

[Edited on 4-10-2006 by Rosco Bodine]
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[*] posted on 3-10-2006 at 23:45


There are several flashes down on the burner, one just a second or two in from the start, several at 13-15 seconds in.

If this is in the US, denatured alcohol is likely to be denatured with methanol, and methyl formate will depart very quickly leaving the ethanol to escape later. Both methyl and ethyl formates ignite rather easily, so don't do that over or near a flame.

I'm a big fan of doing chemistry on the kitchen stove, right next to the cookware. It adds new and exotic flavours to food.
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Rosco Bodine
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[*] posted on 4-10-2006 at 00:04


Another possibility is an adduct compound of the type
described in GB1014071 , which relates to the cocrystallized
addition product of 1 hexamine with 2 ammonium nitrates .
See page 17 and 18 of the patent .

The mole weight of ( 2 ) NH4ClO4 is 234.98
The mole weight of hexamine is 140.19

The ratio of NH4ClO4 to hexamine is 234.98 / 140.19 = 1.68 : 1

not a good match with your stated proportions of 7 : 3 =
2.33 : 1

Anyway it is possible that you have a mixture of the
adduct along with the methylamine perchlorate and
the di and trimethylamine perchlorates and formic acid ,
ammonium formate , formamide ......and here's one to
worry about ...* hydrocyanic acid * ( cyanide gas ) from
the thermal decomposition of the formamide .

So ....good ventilation would probably be a wise precaution
and not a lot of sniffing of the vapors from either the
making or the burning of your mixture , the way you are making it in the video .

All things considered , this is probably not a good procedure
for indoors in the kitchen .

[Edited on 4-10-2006 by Rosco Bodine]
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[*] posted on 4-10-2006 at 04:48


Ok, I'm going to hand over the rest of the experimentation to you, "The experts" who seem to expect all the know hows of possible hazards and precautions and possibilities and stuff.

You all scared me enough to have nothing else to do with it. :)
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Rosco Bodine
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[*] posted on 4-10-2006 at 07:29


Don't misunderstand there being any discouragement of
experimentation , because quite the contrary is true and often it is the only way to learn things , confirm things , or even better to discover things . It is just good sense
to try to know what sort of risks may be present so that
you can use methods which CYA . At lower temperatures
usually everything slows down 50% for each 10C for example , for the reaction rate , so your target condition
for a reaction completion is a more slowly moving target
easier to hit . And many of the reactions for energetic materials involve both explosion hazards and inhalation
hazards .....so these are not unusual risks to be aware of , or to make adjustments to minimize . Doing these
sorts of syntheses outdoors is good practice , if you don't have a regular fume hood in a lab . A box fan sitting on the end of your work table with its intake side
towards your work can produce a draft across the work area to keep fumes out of your face . Portable electric hotplates and crocks and thermostat controlled frypans on the patio table outdoors are better than a kitchen stove indoors . Keep a five gallon bucket full of water
handy , and a hose with a trigger nozzle and a water breaker threaded on the front , the gadget like is used for high volume soft spray watering of potted plants .
If you get splashed with hot and or corrosive materials ,
seconds count and these provide quick access to water .
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[*] posted on 4-10-2006 at 11:51


Hi, I'm the same "Bert" as left the first youtube comment. I'm glad you still have your hands, and any mother or wife connected with the stove in the video has not seen fit to skin you alive.

Does the finished product solidify if allowed to cool to room temperature? You will note the use of guar gum and cross linking agents in the commercial water gel explosives described in Rosco Bodine's linked PDF. I'm wondering if you dried the product out to the point it would solidify without these. I have seen procedures for MMAN calling for distilling out the remaining water under vacuum and casting the remaining MMAN directly into containers.

I have used both ammonium perchlorate and hexamine in the production of colored stars for pyrotechnic uses. I hope this tidbit doesn't make it even more difficult to obtain them-
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[*] posted on 4-10-2006 at 12:56


No, it appears to retain it's syrupy sonsitency in room temperature and a bit more solid in the freezer but still melable.

Thanks for the advice Rosco.

[Edited on 4-10-2006 by iv81]
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Rosco Bodine
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[*] posted on 4-10-2006 at 13:30


You ever burned any of those paper wrapped sparklers that are spiral wrapped tissue on a bamboo splint about
the same as used for the stick on bottle rockets ?

When the sparkler burns about two thirds down , there
is an erruption of popping sparkling stars , which reminds me a lot of this composition in the video .

Does anybody know what is the composition for those
little popping flashbulb star granules/prills that are in the paper wrapped sparklers ?
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[*] posted on 4-10-2006 at 13:52


Probably crackling microstars...

I'd think you'd know that. You do more explosives than pyrotechnics?

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Rosco Bodine
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[*] posted on 4-10-2006 at 14:46


Yeah ....I'm more of an ops man than a pyro .

crackling microstars huh , sounds about right .....
add a bunch of them together and you might get more than a crackle :D ....so what's in 'em ?

[Edited on 4-10-2006 by Rosco Bodine]
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[*] posted on 4-10-2006 at 15:43


Crackling micro stars are Lead tetroxide or Bismuth trioxide with Magnesium/Magnalium bound with nitrocellulose lacquer. Some formulations also contain black Copper oxide. The actual mechanism that causes them to explode is unknown.

Typical formulations-

Bismuth trioxide 75
Magnalium, -200 mesh 15
Black copper oxide 10
Aluminum, 200 mesh atomized +5
type cut
solvent 10% NC lacquer


Lead tetraoxide 70
Magnalium, -200 mesh 17.5
Black copper oxide 12.5
Aluminum, 200 mesh atomized +5
type cut
solvent 10% NC lacquer


Additionaly, some colored stars containing coarse particles of magnalium will crackle as the magnalium particles melt.


[Edited on 4-10-2006 by Bert]

[Edited on 4-10-2006 by Bert]
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[*] posted on 4-10-2006 at 16:32


Quote:
Originally posted by Bert
The actual mechanism that causes them to explode is unknown.


One of these odd things indeed, especially considering the high densities required for these microstars to work properly. While for flashpowder the opposite is true...

Somehow it must be surface related, since larger microstars behave much different and rarely explode as a whole. The burning outerlayer may be able to "cook off" a certain volume, given that that inner volume to be heated is not too large or it will not reach this critical temperature...

[Edited on 5-10-2006 by nitro-genes]
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