| Pages:
1
2 |
phendrol
Harmless
Posts: 34
Registered: 13-6-2012
Member Is Offline
Mood: sock puppet
|
|
Methylamine HCl with a pipe bomb
Hello
I'm thinking about preparing methylamine hcl with a pipe bomb. I made it some time ago from hexamine with much success, but the pipe bomb route seems
to be even less labour intensive. The only thing that discourages me, is that there are chances of a serious accident while attempting the synthesis.
The recipe is as follows:
400 ml of methyl alcohol with 535 grams of ammonium chloride, 400 ml of water, and 2.5 grams of ferric chloride are heated in a 2 l pipe bomb to 300
C for two hours.
Now could anyone give me a clue on the pressure inside the vessel? Will a steel pipe, with 2mm thick walls survive it?
|
|
|
haroldramis
Harmless
Posts: 21
Registered: 6-1-2012
Member Is Offline
Mood: No Mood
|
|
reference please?
|
|
|
hyfalcon
International Hazard
Posts: 1003
Registered: 29-3-2012
Member Is Offline
Mood: No Mood
|
|
I wouldn't want to be around it. Just water alone superheated can generate quiet a force in and of itself. If you were standing in the wrong spot
when it failed, well, it wouldn't be good.
|
|
|
chemrox
International Hazard
Posts: 2961
Registered: 18-1-2007
Location: UTM
Member Is Offline
Mood: LaGrangian
|
|
If hexamine was too much hassle I wonder about making the pipe bomb. Surely you wouldn't just hop down to the plumbers supply and buy galvanized
steel parts?
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
|
|
|
bbartlog
International Hazard
Posts: 1139
Registered: 27-8-2009
Location: Unmoored in time
Member Is Offline
Mood: No Mood
|
|
Vapor pressure of methanol at 300C is about 2000 psi. Whether a pipe with 2mm thick walls would survive it depends on the type of steel and the
diameter of the pipe, among other things; in general I would worry more about failure at the ends/caps/flanges. And I would recommend the Hofmann
degradation of acetamide as a less dangerous and more easily controlled method of synthesis.
The less you bet, the more you lose when you win.
|
|
|
phendrol
Harmless
Posts: 34
Registered: 13-6-2012
Member Is Offline
Mood: sock puppet
|
|
It's taken from US patent 2085785. I think I will try it in about a week or two. You can be sure I'll post my results.
|
|
|
turd
National Hazard
Posts: 800
Registered: 5-3-2006
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by phendrol  |
400 ml of methyl alcohol with 535 grams of ammonium chloride, 400 ml of water, and 2.5 grams of ferric chloride are heated in a 2 l pipe bomb to 300
C for two hours.
Now could anyone give me a clue on the pressure inside the vessel? Will a steel pipe, with 2mm thick walls survive it? |
 Are you completely out of your mind? Switch to theoretical chemistry, at least
you won't hurt yourself/others.
|
|
|
haroldramis
Harmless
Posts: 21
Registered: 6-1-2012
Member Is Offline
Mood: No Mood
|
|
Thanks for the info on that Patent. Out of all the amine making documents Ive seen, i never saw that one before. Looks like quite a gem if it works
as advertised.
Ill be anxiously awaiting your results.
|
|
|
ItsAChitzen
Harmless
Posts: 47
Registered: 18-6-2012
Location: A Sauna
Member Is Offline
Mood: lulz
|
|
...
Wtf? There are better ways to make this. Also, it is cheap as fuck. Also, it is a Precursor. You know the one I mean. LoL to you and those
helping you...
|
|
|
chemrox
International Hazard
Posts: 2961
Registered: 18-1-2007
Location: UTM
Member Is Offline
Mood: LaGrangian
|
|
| Quote: Originally posted by phendrol | | It's taken from US patent 2085785. I think I will try it in about a week or two. You can be sure I'll post my results. |
This patent number yielded something called "Tag Package" What is the correct number?
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
|
|
|
phendrol
Harmless
Posts: 34
Registered: 13-6-2012
Member Is Offline
Mood: sock puppet
|
|
| Quote: | | Wtf? There are better ways to make this. Also, it is cheap as fuck. Also, it is a Precursor. You know the one I mean. LoL to you and those helping
you... |
It's not a controlled substance where I live, and if you know better ways to make this, please share...
| Quote: | | This patent number yielded something called "Tag Package" What is the correct number? |
http://www.freepatentsonline.com/2085785.pdf
|
|
|
ItsAChitzen
Harmless
Posts: 47
Registered: 18-6-2012
Location: A Sauna
Member Is Offline
Mood: lulz
|
|
If it isn't a controlled substance, I would buy it from a manufacturer...
[Edited on 19-6-2012 by ItsAChitzen]
|
|
|
madcedar
Hazard to Others
Posts: 116
Registered: 10-9-2009
Member Is Offline
Mood: No Mood
|
|
Since nothing interesting comes up when using the sciencemadness search engine, I think you'll find the links below useful.
Acetamide to Methylamine
http://www.sciencemadness.org/talk/viewthread.php?tid=7410
Good way to Methylamine HCl?
http://www.sciencemadness.org/talk/viewthread.php?tid=1261
Methylamine Purification
http://www.sciencemadness.org/talk/viewthread.php?tid=9139
Cheers
PS: Oh by the way, the main problem with using the bomb is that (from reading between the lines in the patent) it seems the major product of the
reaction will be the diamine and not the mono-amine you are after.
[Edited on 19-6-2012 by madcedar]
|
|
|
turd
National Hazard
Posts: 800
Registered: 5-3-2006
Member Is Offline
Mood: No Mood
|
|
No, the main problem with "using the bomb" is that it has an appreciable chance of killing or seriously hurting him. If you lack the equipment and
experience, then you don't do high pressure reactions. Period. Aside from the economic stupidity - for the price of a real autoclave you can buy
MeNH2.HCl lasting more than a lifetime.
|
|
|
madcedar
Hazard to Others
Posts: 116
Registered: 10-9-2009
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by turd | | No, the main problem with "using the bomb" is that it has an appreciable chance of killing or seriously hurting him. If you lack the equipment and
experience, then you don't do high pressure reactions. Period. Aside from the economic stupidity - for the price of a real autoclave you can buy
MeNH2.HCl lasting more than a lifetime. |
100% correct.
One more reference for you Phendrol that seems easy and safe:
http://www.erowid.org/archive/rhodium/chemistry/methylamine....
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I would also like to mention another similar "pipe bomb" reaction; one that could be used to convert urea into guanidine:
By heating urea, ammonium chloride, and aluminum sulfate together with ammonia under pressure, guanidine can be obtained. The reaction products are
boiled with an ammonium hydroxide solution to precipitate out the aluminum hydroxide. The remaining clear filtrate contains guanidine hydrochloride,
ammonium sulfate, unreacted urea, and unreacted ammonium chloride. Using equimolar ammounts of NH4Cl and urea, with one third of a mole aluminum
sulfate for every mole of urea, heated to 275degC, and subjected to 6.8 atmospheres of pressure, the yield of guanidine (relative to initial urea) was
28% after 30 minutes, and 34% after two hours. Using excess NH4Cl increased the yields further.
|
|
|
BooMMaker
Harmless
Posts: 1
Registered: 14-8-2012
Member Is Offline
Mood: No Mood
|
|
HMTD isn't a bad choice either, if you want to stick with hex.
|
|
|
SM2
Hazard to Others
Posts: 359
Registered: 8-5-2012
Location: the Irish Springs
Member Is Offline
Mood: Affect
|
|
Well, my personal favorite, is to reduce nitromethane in an acidic (HCLaq) environment using activated aluminum. Clean up your almost pure white
xtals of methyl-ammonium chloride. If you need Ethylamine HCL, just use Remove, artificial nail remover by Gena labs.
|
|
|
#maverick#
Hazard to Others
Posts: 209
Registered: 7-4-2011
Member Is Offline
Mood: hybridised
|
|
Interesting concept, but as others have said, dangerous, stupid and there are easier ways, ive personally made methylamine using this method http://www.sciencemadness.org/talk/viewthread.php?tid=7410
[Edited on 18-8-2012 by #maverick#]
|
|
|
unionised
International Hazard
Posts: 5102
Registered: 1-11-2003
Location: UK
Member Is Offline
Mood: No Mood
|
|
Am I the only one who thought
NH4Cl ---> NH3 +HCl
Fe + 2HCl --> FeCl2 + H2
And
2 FeCl3 + Fe ---> 3 FeCl2
So there's less metal holding the pressure and more gas (the hydrogen) exerting that pressure.
This doesn't seem a good idea to me.
|
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
Glass bombs and ZnCl2 were tried first here:
http://www.sciencemadness.org/talk/viewthread.php?tid=1261&a...
"they failed"
|
|
|
zed
International Hazard
Posts: 2277
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
The conditions initially proposed would probably require the use of a Parr-type high pressure reactor. If you don't have one, small diameter
stainless steel tubing can withstand very high pressures.
We have had similar discussions on producing Diethylamine by such procedures. Except that, ammonium acetate is used is used as a starting material,
rather than ammonium chloride. My intuition is, that ammonium acetate might be less corrosive.
|
|
|
beatle_guce
Harmless
Posts: 6
Registered: 14-7-2012
Member Is Offline
Mood: No Mood
|
|
just use one of those high pressure co2 tanks for paint ball. I think they have ones thats good for 3000-4000psi youll have to expel all the gas first
then muscle a monkey wrench to open it up, then clean out the interior, load it up and close
|
|
|
UnclearReactor
Harmless
Posts: 9
Registered: 11-1-2008
Location: Eastern US
Member Is Offline
Mood: No Mood
|
|
The paintball tank is NOT rated at 300° C. It's much weaker when that hot. The aluminum it is made of will react and corrode (but so would the zinc
on a galvanized pipe, the iron in a black Iron pipe, not to mention contaminating the reaction). This is a recipe for disaster.
|
|
|
Mildronate
Hazard to Others
Posts: 428
Registered: 12-9-2009
Member Is Offline
Mood: Ruido sintetico
|
|
methylamine synth
I read in Festers Advanced Techniques of Clandestine Psychedelic & Amphetamine Manufacture book, methylamine synth from MeOH and NH4Cl in high
preasure, does it really work?
Attachment: metila.pdf (1.6MB)
This file has been downloaded 5733 times
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
